英文化学报告标准用语

STANDARDIZED PHRASE FOR REPORT/英文报告标准用语l Process Description/工艺描述No.Unit OperationsProcess description in ChineseProcess description in English1Instrument/Equipment preparation仪器/设备准备装有机械搅拌(或磁力搅拌)，加料漏斗，温度计(或分水器，干燥管)的3L三口瓶A 3L three-necked round bottom flask equipped with mechanical stirrer (or magneticstirrer), addition funnel and thermometer (or Dean-Stock; drying tube)反应中所用的所有瓶子，真空条件下加热30min，氮气吹扫10min。All flasks used in the reaction were heated under vacuum for 30 minutes and purged with nitrogen for 10 minutes.将500L高压釜通氮气至0.40.5MPa。若0.51h内压力无变化，则气密性良好。A 500L autoclave reactor was filled with nitrogen to increase the pressure to 0.40.5MPa. If the pressure had no change within 0.51h, then the air-tightness of the autoclave reactor was good.将500L搪瓷釜抽真空到60oC用氮气烘68h，然后降温到2025oC。A 1000L titanium reactor was dried at 60oCwith hot nitrogen for 68h, then cooled to 2025oC.2Charging/投料Order/顺序向瓶中加入A 10ml(1mol)，B (2 g, 2mol) and C (50 ml )The flask was charged with A (10 ml, 1 mol), B (2 g, 2mol) and C (50 ml )依次加入D (10 g, 1 mol) and E (20 ml)D (10 g, 1 mol) and E (20 ml) were added in turn向A(10ml, 1 mol)和B (2 g, mol)的C(50ml)溶液(体系或悬浮液)中，依次加入D (10 g, 1 mol) 和 E (20 ml)D (10 g, 1 mol) and E (20 ml) were added into a solution (mixture or suspension) ofA (10 ml, 1 mol) and B (2 g, mol) in C (50 ml) in turnWay/方式氮气保护下，控温2030oC，通过固体加料漏斗一次性向100L搪瓷釜中加入A (40.0kg, 10.0mol)Under the protection of nitrogen, A(40.0kg, 10.0mol) was added into a 100L glass-lined reactor in one portion via the solid additional funnel while maintaining the temperature at 2030oC控温2030oC， 向500L白钢釜中， 分四批加入A (10.0kg, 10.0mol)，每批2.5kg，间隔时间为510minA(10.0kg, 10.0mol) was added to a 500L stainless steel reactor in four portions (2.5kg4) at interval of 510min while maintaining the temperature at 2030oC将D (10 g, 1 mol) 分批加入，1h加完。D (10 g, 1 mol) was added in portions during a period of 1 h.将D (10 g, 1 mol) 分批加入，1h内加完。D (10 g, 1 mol) was added in portions within 1 h.2Charging/投料Way/方式控温2030oC， 用真空向干燥洁净的100L搪瓷釜中抽入114260的乙酸乙酯溶液(外标折算后为50.0kg 114260)。Maintaining the temperature at 2030oC, solution of 114260 in ethyl acetate (50.0kg 114260 corrected by wt%) was added by vacuum to a clean and dried 100L glass-lined reactor控温2030oC，用氮气压入A(100kg, 101mol)，开动搅拌，A(100kg,101mol) was added(charged) by nitrogen at 2030oC and then the stirrer was started.控温2030oC，用真空抽入A(100kg, 101mol) Maintaining the temperature at 2030oC, A (100kg,101mol) was added(charged) by vacuum.控温2030oC，用泵打入A(100kg, 101mol)A(100kg,101mol) was added(charged) by pump while maintaining the temperature at 2030oC将正丁基锂或硼烷/四氢呋喃溶液(10 ml, 1 mole, 2.5 M in 己烷)，通过管路导入滴加漏斗或A的B溶液中。A solution of BuLi or BH3/THF (10 ml, 1 mole, 2.5 M in hexane) was cannulated intoaddition funnel or into a solution A in solvent B通过插管，滴加漏斗或针筒，将正丁基锂或硼烷/四氢呋喃溶液(10 ml, 1 mole, 2.5 M in 己烷)，通过管路导入滴加漏斗或A的B溶液中，5h加完。A solution of BuLi or BH3/THF (10 ml, 1 mole, 2.5 M in hexane) was added into asolution of A in solvent B via cannula, dropping funnel or syringe over a period of 5h3Add dropwise滴加控温1015oC，通过50L滴加罐(高位瓶或恒滴)向体系中滴加D (101kg, 10 mol)，滴速为1520kg/h。D (101g, 10mol) was added dropwise into the mixture through (via) 50L additional vessel (or carboy or constant pressure funnel) at a rate of 1520kg/h while maintaining the temperature at 1015oC.控温10oC(或保持微回流或保持内温1030oC)，氮气保护下，(通过加料漏斗或针筒)滴加D (10 g, 1 mol) 的 E (20 ml)溶液。a solution of D (10 g, 1 mol) in E (20 ml) was added dropwise (via addition funnelor syringe) at 10oC (or while maintaining gentle reflux; while keeping inner temperature between 10oC 30oC) under nitrogen4Heat升温将体系升温至1520oC，升温速度510oC/hThe mixture was heated to 1520oC at the rate of 510oC/h.用汽水混合器将体系升温至5060oC。The mixture was heated to 5060oC by the steam-water mixing heating.5Cool降温将体系降温至1520oC，降温速度510/hThe mixture was cooled to 1520oC at the rate of 510oC/h.用外浴乙醇/液氮将体系降温至-70-75oCThe mixture was cooled to -70-75oC by ethanol/liquid nitrogen6Maintain保温将体系于1520oC保温搅拌0.5h。The mixture was stirred at 1520oC for 0.5h。7Reflux回流体系于7882oC回流3h。The mixture was refluxed at 7882oC for 3h.8Exchange/置换控温2030oC，将氮气通入液面下置换体系10次，每次通氮气至0.2MPa，然后排空至常压；再液面下通氢气置换体系5次，每次通氢气至0.2MPa，然后排空至常压。（高压反应中用到）The mixture was exchanged with nitrogen under liquid level for 10 times. The pressure was increased to 0.2MPa with nitrogen and pumped down to normal pressure each time. And then the mixture was exchanged with hydrogen under liquid level for 5 times. The pressure was increased to 0.2MPa with hydrogen and pumped down to normal pressure each time. During exchanging, the temperature of mixture was controlled at 2030oC9React反应Type/类型无溶剂反应：将A (1 g, 1 mol) and B (1 g, 1 mol)溶于溶剂C中，蒸干后，于50oC加热2小时。A (1 g, 1 mol) and B (1 g, 1 mol) were dissolved in solvent C, evaporated to dryness and heated at 50oC for 2h。催化量的反应：于0oC，加入A (20 ml, 142 mmol)和催化量B（1微量或两滴），加入C(4.549 g, 46.4 mmol)的D (120ml)溶液中。A (20 ml, 142 mmol) and catalytic amount (a trace amount or two drops) of B were added into a solution of C (4.549 g, 46.4 mmol) in D (120mL) at 0oC闷罐反应或封管反应：控温T=40oC，P=0.5MP ，A(1g, 1mol)的饱和氨水（或其他气体如：一氧化碳、二氧化碳、硫化氢）乙醇(1ml)溶液在50ml封管或闷罐/高压釜中搅拌5小时。A solution of A (1g, 1mol) in ethanol (x ml) saturated with NH3 (or other gas such as: CO,CO2, H2S) was stirred under 0.5MPa at 40oC for 5hrs in a 50 ml of sealed tube or autoclave.A(1g, 1mol) 的饱和氯化氢甲醇(1ml) 溶液在20oC搅拌。A solution of A (1g, 1mol) in methanol (1ml) saturated with HCl was stirred at 20oC.控温20oC，向A(1g, 1mol)的甲醇(1ml)溶液中通臭氧15min。然后通氮气除臭氧，再于20oC加入Me2S (5ml)。Ozone was bubbled into a solution of A (1g, 1mol) in MeOH (1ml) at 20oC for 15minutes. After excess O3 was purged by N2, Me2S (5ml) was added at 20oC.9React反应Type/类型A(1g, 1mol)和B(1g, 1mol)的C(1ml)溶液在30oC下通气体0.5小时。Gas was bubbled into a solution of A (1g, 1mol) and B (1g, 1mol) in solvent C (1ml) at 30oC for 0.5h.控温10oC，D(1g, 1mol) 加入到A(1g, 1mol)的B(5ml)和C(10ml)溶剂混合液（或B和C的混合溶剂）中，反应体系搅拌（回流或加热）两小时。To a solution of A (1g, 1mol) in a mixture of solvent B (5ml) and solvent C (10ml) (or a mixed solvent of B and C) was added D (1g, 1mol) at 10oC, the reaction mixture was allowed to stir (reflux or heat) for 2h.向A(1g, 1mol)的丙酮水溶液（丙酮:水=10：1）中加入B (1g, 1mol)，再加入C(1g, 1mol)，反应体系搅拌（回流或加热）五小时。To a solution of A (1g, 1mol) in 10: 1 aqueous acetone (1ml) was added B (1g, 1mol) followed by addition of C (1g, 1mol), the reaction mixture was allowed to stir (reflux or heat) for 5hrs.将A和B溶于苯或甲苯，体系回流1h，共沸带水。A (x g, x mol) and B (x g, x mol) in benzene or toluene (x mL) were refluxed for xh with azeotropical removal of water.将A、B和甲苯磺酸的甲苯溶液加热回流，用分水器除水。A mixture of A, B and TsOH.H2O (56.91 g, 0.3 mol) in toluene (400 mL) was heated toreflux and remove water by Dean-Stark trap.氮气保护下，向A的乙醇溶液中加入Pd-C或Ra-Ni或Pd(OH)2/C。悬浮液真空下除氧，再通几次氢气。To a solution of A (x g, x mol) in EtOH (x mL) was added Pd-C or Ra-Ni or Pd(OH)2/C (10%,x g) under N2. The suspension was degassed under vacuum and purged with H2 several times.体系于5 psi ，20oC搅拌氢化1h。氢化瓶或高压釜The mixture was stirred under H2 (5 psi) at 20oC for 1h. 体系于20oC搅拌氢化1h。常压氢化如气球反应The mixture was stirred under H2 balloon at 20oC for 1h.A和Ra-Ni的乙醇溶液在室温、50Psi氢气压力下氢化2h。A mixture of A (x g, x mol) and Ra-Ni (x g) in EtOH (x ml) was hydrogenated under50 Psi of hydrogen pressure for 2h at room temperature.Condition or process/条件或过程反应体系(溶液或悬浮液)于5oC搅拌2hrs后，于室温保温2hrs(或过夜)。The reaction mixture (solution or suspension) was stirred at 5oC for 2h and then kept at room temperature (or ambient temperature) for another 2h (or overnight)反应体系(溶液或悬浮液)于60oC回流2hrs(或过夜)。The reaction mixture (solution or suspension) was refluxed at 60oC for 2h (or overnight)9React反应Condition or process/条件或过程反应体系(溶液或悬浮液)容许回流2hrs(或过夜)。The reaction mixture (solution or suspension) was allowed to reflux (or heat to reflux) for 2h (or overnight)反应体系(溶液或悬浮液)容许回温2hrs后， 回流2hrs(或过夜)The reaction mixture (solution or suspension) was allowed to warm to temperature during 2h and reflux for 2h (or overnight)State or Endpoint of reaction/反应状态或终点反应通过TLC(石油醚：乙酸乙酯=4：1)，LC-MS，液相或核磁确认完成（为完成或杂乱的）。The reaction was complete (incomplete or messy) detected (determined or confirmed) by TLC (PE/EtOAc 4:1), LC-MS, HPLC or NMRTLC(石油醚：乙酸乙酯=1：1)或液相(107757-088-1)显示反应结束。TLC (PE:EtOAc=1:1) or HPLC (107757-088-1) showed or indicated that the reaction was complete.TLC(石油醚：乙酸乙酯=1：1)或液相(107757-088-1)显示起始原料完全消耗。TLC (PE:EtOAc=1:1) or HPLC (107757-088-1) showed the starting material was consumed completely.TLC(石油醚：乙酸乙酯=1：1)或液相(107757-088-1)显示根本没有反应或大部分原料剩余。TLC (PE: EtOAc =1:1) or HPLC (107757-088-1) showed the reaction didnt work at all or most of starting material was still remained.起始原料完全消耗，但经MS (106657-078-1) 或LC-MS (106657-078-1)检测，没有预期的产物。The starting material was consumed completely, but no desired compound was detected or determined by MS (106657-078-1) or LC-MS (106657-078-1).TLC显示有几个点Several spots were shown on TLC.经MS (106657-078-1) 或LC-MS (106657-078-1)或 HPLC (106657-078-1) 或TLC (石油醚：乙酸乙酯=1：1).检测，只有很少量的预期产物。Only a trace amount of desired compound was detected by MS (106657-078-1) orLC-MS (106657-078-1) or HPLC (106657-078-1) or TLC (PE:EtOAc=1:1).由于收率低或溶解性不好，通过层析或制备的高效液相色谱仪，不能分离或纯化预期化合物，。The desired compound could not be isolated, separated or purified by chromatography or prep. HPLC due to poor yield or poor solubility.通过1H NMR (106675-010-2) or MS确认，得到(或分离)的不是预期化合物，反应失败。1H NMR (106675-010-2) or MS confirmed the obtained (or isolated) compound is not the desired compound. The reaction failed.9React反应Scaling up technic in Asymchem/放大工艺中体系于5055oC反应，12h后， 每12h取样一次HPLC跟踪，直至化合物A含量1%且连续两次取样化合物A含量变化0.5%。若连续两次取样化合物A含量变化0.5%且化合物A含量1%，则补加化合物BThe mixture was stirred at 5055oC. 12h later, the reaction was monitored by HPLC every 12h. The reaction was considered completion when the content of compound A was 1% and the change of compound A content between consecutive samples was 0.5%. If change of compound A content between consecutive samples was 0.5% and the content of compound A was still 1%, extra compound B was added.体系于5055oC搅拌反应，12h后， 每12h取样一次HPLC跟踪，直至113443相对于乙苯含量0.1%The mixture was stirred at 5055oC. 12h later, the reaction was monitored by HPLC every 12h. The reaction was considered as complete when the peak area of 113443 0.1% relative to ethyl benzene10Sampling method取样方法(由于终产品报告中，取样方法用一般现在时，故此处也用一般现在时)从反应体系(溶液或悬浮液)通过滴管或注射器取样。处理完毕后，通过TLC, LC-MS or HPLC检测反应Take sample from the reaction mixture (solution or suspension) by dropping tube or syringe. After workup, check the reaction via TLC, LC-MS or HPLC etc.用取样器取滤液5ml，直接送样检测液相外标Take 5ml filtrate with the sampler; send to be analyzed wt% by HPLC directly.用药勺取滤饼2g，直接送样检测液相纯度Take 2g filter cake with the medicinal ladle; send to analyze its purity by HPLC directly.用取样器取体系23ml，打入5ml纯净水中，用2ml乙酸乙酯萃取后，有机相送液相Take 23ml mixture with the sampler, add it into 5ml purified water. After extract with 2ml ethyl acetate, Send the organic phase to be analyzed by HPLC. 用取样器取体系5ml，静置后分液，有机相用TLC检测(乙酸乙酯:环己烷=3:7)Take 5ml mixture with the sampler, hold and then separate. Send the organic phase to be analyzed by TLC (ethyl acetate: n-hexane=3:7)11Quench 终止当反应体系(溶液或悬浮液)回温至-5oC(或室温)，将A水溶液滴加到反应体系中。An aqueous solution of A (10 ml) was added dropwise into the reaction mixture once the reaction mixture (solution or suspension) was allowed to warm (or cool) to -5oC (or room temperature or ambient temperature)热的(或冷的)反应体系(溶液或悬浮液)倒入水(冰水)中或浇到冰上。The hot (or cold) reaction mixture (solution or suspension) was poured into water (icewater) or poured onto ice11Quench 终止反应体系(溶液或悬浮液)减压浓缩(或蒸馏)去除甲醇(四氢呋喃或N,N-二甲基甲酰胺)或过多的氯化亚砜(试剂)。用溶剂稀释反应体系后，倒入水(冰水)中或浇到冰上。The reaction mixture (solution or suspension) was concentrated (distilled) under reduced pressure (in vacuum) to remove MeOH (THF; DMF etc.) or excess SOCl2 (reagent). Then the reaction residue (or the residual) was diluted with solvent and poured into water (ice water) or poured onto ice将反应体系转至装有100.0kg纯净水和100.0kg冰的1000L搪瓷釜中冰解。The reaction mixture was quenched with mixture of purified water (100.0kg) and ice (100.0kg) in a 1000L glass-lined reactor.控温1015oC，通过50L高位瓶或滴加罐向反应体系中滴加20kg纯净水终止反应滴速为510kg/h。Purified water (20.0kg) was added dropwise via a 50L carboy (additional vessel) to quenched the reaction while maintaining the temperature at 1015oC. The addition rate was 510kg/h.12Adjust pH调pH值向滤液中滴加5%氢氧化钠溶液，调节pH=89，滴速为1015kg/h5% sodium hydroxide solution was added dropwise into the filtrate to adjust pH=89at a rate of 1015kg/h.控温2030oC，用20%盐酸溶液调节体系pH=34The mixture was adjusted to pH=89 with 20% hydrochloric acid at 2030oC.13Filter过滤/抽滤/离心将体系过铺有45cm厚硅胶的700压滤罐。The mixture was filtered by the700 nutsche filter which was pre-loaded with 45cm silica gel.控温2030oC，将体系转移至700压滤罐压滤，用5kg无水乙醇淋洗滤饼。滤液通过流体过滤器压至洁净干燥的300L搪瓷釜中。Maintaining the temperature at 2030oC, the mixture was filtered with700 nutsche filter and the filter cake was rinsed with anhydrous ethanol (5.0kg). The filtrate was transferred by nitrogen through the in-line fluid filter into the 300L glass-lined reactor将体系通过500抽滤缸抽滤The mixture was filtered with the500 vacuum filter.将体系转入SS800离心机中分批离心The mixture was filtered with SS800 centrifuge in portions14Prepare solution/配溶液向2个桶中，分别加入10.0kg氢氧化钠和25.0kg纯净水，搅拌至固体全溶后待用。Sodium hydroxide (10.0kg) and purified water (25.0kg) were averagely added to two drums and stirred until the solid dissolved completely.向1000L搪瓷釜中抽入100.0kg 纯净水和100.0kg 95% 乙醇，搅拌均匀。Purified water (100.0kg) and 95% ethanol (100.0kg) were added by vacuum into a 1000L glass-lined reactor. It was stirred until homogenous.15Extract萃取水相用乙酸乙酯萃取三次。每次用17kg乙酸乙酯，搅拌15min，静置30min后分液The aqueous phase was extracted with ethyl acetate(17kg3). Each time it stirred for 15min and held for 30min before separation.残留液在乙酸乙酯(100 ml)和1N盐酸水溶液(50 ml)盐酸混合物中进行分离，分离的有机相用水洗涤，用硫酸钠(硫酸镁)干燥后，蒸干。The residue was partitioned between ethyl acetate (100 ml) and 1N aq. HCl (50 ml).The separated organic layer was washed with water, dried over (Na2SO4 or MgSO4) and evaporated to dryness.终止毕，将反应体系倒入分液漏斗中分液。After quenching the reaction, the reaction mixture was poured into separatory funnel and separated.水相用有机溶剂 (40ml) 萃取两次(或X次)。合并的有机相用水溶液A(50ml)或水洗涤，用无水硫酸钠或硫酸镁干燥。The aqueous layer (or phase) was extracted with organic solvent (40 ml) twice (or Xtimes). The combined organic layers were (or the organic layers were combined and) washed with an aqueous solution of A (50 ml) or water and dried over Na2SO4 or MgSO4.合并的水相用溶剂(40ml)萃取两次(或X次) 去除中性杂质。水相用盐酸水溶液(或碳酸氢钠)调酸(或调碱)到pH= X后，用有机溶剂萃取。The combined aqueous layers were extracted with solvent (40 ml) twice (or X times) to remove neutral impurities. The aqueous phase was acidified (or basified) with aqueous HCl (or NaHCO3) till PH = X and extracted with organic solvent.合并的有机相用A的水溶液(50 ml)或水洗涤后，用硫酸钠或硫酸镁干燥。The combined organic layers were (or the organic layers were combined and) washedwith an aqueous solution of A (50 ml) or water and dried over Na2SO4 or MgSO4.16Concentrate浓缩滤液于T30oC，P -0.08MPa减压浓缩至无馏分（体系约剩余30L）.The filtrate was concentrated at 30oC under reduced pressure (P -0.08MPa) until no more distillate was observed (approximately remained 30L).体系于4050oC，常压浓缩至体系剩余5060L。The mixture was concentrated at 4050oC under normal pressure until 5060L mixture remained.体系于T50oC，P -0.08MPa减压浓缩至无馏分（体系约剩余30L）。向体系中补加20.0kg甲基叔丁基醚，继续于T30oC，P -0.08MPa减压浓缩至体系剩余约5060L。重复补加操作和减压操作直至乙酸乙酯含量1%The mixture was concentrated at 50oC under reduced pressure (P -0.08MPa) until no more distillate was observed (approximately remained 30L). 20.0kg MTBE was added into the mixture and continued to concentrate at 50oC under reduced pressure (P -0.08MPa) until 5060L mixture remained. The addition and concentration were repeated until the content of ethyl acetate 1%.向体系中抽入20.0kg甲基叔丁基醚，于30oC，P -0.08MPa减压浓缩至乙酸乙酯含量1%。20.0kg MTBE was added into the mixture. Then it was concentrated at 30oC under reduced pressure (P -0.08MPa) until content of ethyl acetate 1%.滤液通过滤纸或者硅藻土垫过滤后，有机层或者萃取层在减压条件下或者真空中浓缩或蒸发干后得到一种油状物（泡沫）（可以固定成型）或者白色固体。After filtration via filter paper or celite pad, the organic layer (or extract) was concentrated under reduced pressure (or in vacuum) or evaporated to dryness to provide (afford; give or yield) an oil (or foam) (which solidified on standing) or a white solid.有几层或者萃取层被压滤，再在减压或真空条件下浓缩或者蒸发干得到A (10 g, 0.5 mole)，是一种油状物或泡沫（可以固定成型）或是白色固体。The organic layer (or extract) was filtered and concentrated under reduced pressure (or in vacuum) or evaporated to dryness to provide (afford or give) A (10 g, 0.5 mole) an oil (or foam) (which solidified on standing) or a white solid.通过蒸发或者浓缩去除溶剂后，得到A(10 g, 0.5 mole)，是一种油状物或泡沫（可以固定成型）或是白色固体。After removal of solvent by evaporation or concentration, A (10 g, 0.5 mole) was obtained (or prepared) an oil (or foam) (which solidified on standing) or a white solid.二氯甲烷的提取液蒸干后，然后与甲苯交换除去残留的二氯甲烷。The extract in CH2Cl2 was evaporated to dryness and then swapped with toluene toremove residual CH2Cl2.17Distill蒸馏将体系于3040常压蒸馏除去溶剂后，于90120，P6mmHg减压蒸馏。收集3mmHg，100110馏分The mixture was distilled at 3040oC under normal pressure to remove the solvent and then continued to distill at 90120oC under reduced pressure (P6mmHg). The fraction of 100110oC under the reduced pressure of 3mmHg was collected.18Rinse淋洗用10kg乙酸乙酯淋洗滤饼The filter cake was rinsed with 10kg ethyl acetate.用甲醇淋洗滤饼至TLC检测无产品残留，每次甲醇用量10.0kg。The filter cake was rinsed with methanol until no residual product by TLC, methanol (10.0kg) was added each time.19Decolorize/脱色向滤液中加入5kg活性炭，再加入5kg硅胶。升温至回流1h后压滤5kg active carbon was added into the filtrate, followed by the addition of 5kg silica gel. Then the mixture was heated to reflux for 1h. After that, the mixture was filtered.20Crystallization析晶将体系降温至-50，保温搅拌1h析晶The mixture was cooled to -50oC and stirred at this temperature for 1h for crystallization.体系于1520保温析晶，3h后每1-2h取样一次至母液外标1.5%The mixture was maintained at 1520oC for crystallization, 3h later, the mixture was sampled every 1-2h until wt% of the mother liquor1.5%.21Dry干燥/烘料有机相用无水硫酸钠于1530oC搅拌干燥34hThe organic phase was dried with stirring for 34h at 1530oC with anhydrous sodium sulfate滤饼转入800双锥中，于P -0.08MPa，T=3040oC条件下烘料至含水1%The filter cake was transferred into the800 rotary conical dryer. It was dried under the condition of T=3040oC, P -0.08MPa until KF1%.滤饼在烘房中于3040oC烘料至干燥失重1%The filter cake was dried in drying room at 3040oC until LOD1%控温255oC用油泵将体系抽至溶剂残留0.3%The mixture was pulled at 255oC with oil pump until OS0.3%.22Purify/纯化粗品用通过硅胶柱层析纯化，用石油醚：乙酸乙酯=10：1洗脱，得到黄色固体(x g, x%)即产品。The crude product was purified by silica gel chromatography eluted with PE: EtOAc=10:1 to give product (x g, x%) as yellow solid.粗品通过x溶剂(x ml)重结晶纯化。The crude product was purified by re-crystallization (or re-crystallized) from x solvent(x ml).粗品在真空（x oC, x 压力）下进行蒸馏得到无色固体（即纯品x g,x%）The crude product was distilled in vacuum (x oC, x pressure) to afford pure product() as colorless liquid.粗品用柱层析先进行纯化，再用液相色谱或者重结晶进行再纯化得到纯品。The crude product was pre-purified by column chromatography followed by prep.HPLC purification or re-crystallization to afford pure product23Trituration/研碎将残渣用乙醚研碎，过滤，得白色固体。The residue was triturated with ether and filtered to afford a white solid. 24Solidifying by standing/静置固化粗品通过高效液相法纯化，得无色粘稠油状物，静置固化。The crude product was purified