英文实验记录

实验记录常用英文表达句型一、 加料过程常用表述1.添加试剂2.催化量的3.气体保护4.通入气体5.通过双针头导管加料6.通过注射器加料二、 反应过程常用表述1.反应检测2.放置过液3.甲苯/乙醇带水4.氢化反应5.分水器6.反应放热7.微波反应三、 后处理过程常用表述1.过滤2.淬火3.磨碎4.在两相中分开5.静止固化6.在冻干机冻干7.纯化过柱制备HPLC纯化制备TLC纯化重结晶8.调PH9.萃取10.浓缩11.干燥干燥真空干燥四、 部分常见反应现象描述1.加料放热2.反应过程中或者降温有固体析出3.加料不溶解4.反应变粘稠/变色五、 特殊结果叙述1.无进一步处理2.统一和其他批次一起后处理3.检测条件，不需要后处理一、加料过程常用表述1.添加试剂To a mixture (suspension / solution / slurry) of compound 12 (487 mg, 1 mmol) and o-plenylenediamine (948 mg, 6 mmol) in CH2Cl2 (15 ml) being coolen to 0℃ was added the DCC (226 mg, 1.1 mmol).Anhydrous lithium iodide (1.38 g, 10.3 mmol) was added the five portions (dropwise / in one portion / in portions) to a stirred solution of compound 12 (10.90 g, 51.5 mmol) in CH2Cl2 (120 ml).A round-bottom flask was changed with compound 3 (1.75 g, 5.27 mmol), LiCl (1.17 g, 26.3 mmol), DMSO (100 Ml) and H2O (378 ul)分批加入 in portions/portionwise一次性加入 in one portion滴加 dropwise2.催化量的Et3N (20 mL, 142 mmol) and a catalytic amount of DMAP were added the solution of compound 1 (4.549 g, 46.4 mmol) in CH2Cl2（120 ml） at 0℃3.气体保护To a stirred -78 solution℃of trimethylsilyacetylene (4.44g, 45.5 mmol)in THF (10 ml) under argon was added dropwise n-butylithium (1.6M in hexane, 28.25 ml).4.通入气体An ozone-enrichen steam of oxygen was bubbled through a cold (-78) solution of℃compound 9 (128 mg, 1.409 mmol) in CH2Cl2 (5 ml) until it turned light blue. The℃3 . solution was purged with argon at -78 for 10 min to remove the excess O5.通过双针头导管加料The mixture was added to a sulotion of compound 2 (3.00 g, 12.8 mmol) in THF (48 ml) via cannula over a period of 30 min.A solution of compound 29 (100 mg, 0.19 mmol, 1.0 equiv) in dry DMSO (1.5 ml) was cannulated under argon to a vigorously stirred mixture of powered potassium superoxide (62 mg, 0.87 mmol, 4.5 equiv) and 18-crown-6-ether (23 mg, 0.087 mmol, 0.45 equiv) in dry DMSO （0.5 ml）.6.通过注射器加料To a stirred solution of compound 15 (8.61 g, 21.2 mmol) was added a solution of p-toluenesulfonic acid (6.0 g) in CH2Cl2 via syringe over 5 min.7. 反应控温A solution of compound 1 (10 g, 1 mol) in EtOAc (20 ml) was added dropwise (via addition funnel or syringe) to the above mixture at 10 ℃(while maintaining gentle reflux;℃.while keeping internal temperature between 10 ℃ - 30)二、反应过程常用表述1. 常温/回流搅拌℃a.The reaction mixture (solution or suspension) was stirred at 5 for 2 hrs andthen kept at room temperature (or ambient temperature) for another 2 hrs (or overnight)b.The reaction mixture (solution or suspension) was refluxed (or heated to reflux)for 2 hrs (or overnight)℃c.The reaction mixture (solution or suspension) was heated at 60 for 2 hrs (orovernight)d.The reaction mixture (solution or suspension) was allowed to reflux (or heat toreflux) for 2 hrs (or overnight)2. 反应检测a. After 1 h, TLC analysis (CH2Cl2 / hexane 3:1) showed the complete consumption of compound 15.b. The reaction was complete (incomplete or messy) detected by TLC (Petroleum ether/EtOAc = 4:1),LC-MS, HPLC or NMR.3. 放置/过夜The mixture was left standing overnight.The mixture was allowed to stand at room temperature for 1 day.℃The mixture was allowed to stand in a freezer at -15 .4. 甲苯/乙醇带水Compound A (1.97 g, 6.63 mmol) was coevaporated with toluene five times to remove the water. The residue was subjected to toluene azeotrope to give the corresponding acid choride as brown oil. The aqueous portion was concentrated under reduced pressure followed by azeotropic removal of water with absolute EtOH.5. 氢化反应A mixture of compound 1 (190 g, 0.88 mmol) and Raney Ni (20 g) in ethanol (1500 ml) and ethyl acetate (500 ml) was stirred under 1 atm at room temperature for an hour.6. 分水器A mixture of TsOH.H 2O (56.91 g. 0.3 mol) and toluene (400 mL) was heated to reflux to remove water by Dean-Stark trap.7. 反应放热 / 吸热The reaction was exothermic / endothermic .8. 微波反应The sealed vial was irradiated in the microwave on a Biotage Smith Synthesis at 150 for 10 min.℃9. 抽真空The mixture was degassed for 10 min and refilled with N .210. 吸收装置The device for absorbing the evolved hydrogen bromide was attched to the reaction flask. [care!! The reaction evolves HBr and is best connected to a HBr gas trap (bubber containing 1 M NaOH solution)].11.避光反应To the solution which is protected from light was added dropwise Br (3.45 g, 22 mmol) in CH 22Cl 2 (10 mL) over 5 min and the mixture was stirred for 1 h.A mixture of compound 8 (213 mg, 0.186 mmol) and compound 9 (220 mg, 0.279 mmol) was refluxed for 20h under dark in a nitrogen atmsophere.三、后处理过程常用表述1. 过滤The mixture was filtered through a Celite pad, and the filtrate was concentrated to give the crude product.2. 淬火The reaction mixture was quenched by the addition of the saturated aqueous NH4Cl. 3. 磨碎The residue was triturated with ether and filtered to afford a white solid.4. 分液After quenching the reaction, the reaction mixture was poured into separator funnel and separated.5. 在两相中分开The residue was partitioned between ethyl acetate (100 ml) and HCl (1N, 50 ml).The organic layer was washed with water, dried (MgSO4) and evaporated to dryness.Ethyl acetate (100 ml) and HCl（1 M aq, 50 mL）were added to the residue, and the layers were separated.6. 静止固化The crude product was purified by prep-HPLC to give compound 4 as colorless thick oil, which was solid i fied on standing.7. 在冻干机冻干The white solid was re-crystallized from water, dried by hyophilization to give a white solid.7.纯化7.1 过柱The crude produt was chromatographed on silica gel (CH2Cl2 / MeOH 20:1→10:1→5:1) to give the compond 8 (0.282 g, 51%) as a white solid.The crude product was purified by column chromatography on silica gel eluted with (CH2Cl2 / MeOH 20:1→10:1→5:1) to give the compound 8 (0.282 g, 51%) as a white solid.7.2 制备HPLC纯化Be purified by prep-HPLC to afford/give/yield7.3 制备TLC纯化Be purified by prepare TLC to afford/give/yield7.4 重结晶Recrystallized from8.调PHThe pH was adjusted to around 9 by progressively adding solid NaHCO3.The mixture was adjusted to pH 9 with solid NaHCO3.酸化: be acidified to 碱化: be basified to 中和: be neutralized9.萃取The aqueous layer was extracted with ethyl acetate (100 mL×4).10.浓缩The mixture was evaporated to afford the crude product.The mixture was concentrated afford the crude product.The solvent was removed to afford the crude product.11.干燥11.1 常规干燥The organic layer was dried over , and concentrated.MgSO411.2 真空干燥The precipitate was filtered and dried (in/under vacumm; under reduced pressure).四、部分常见反应现象表述1.加料加热A gentle reflux appeared throughout the addition.The temperature was increased from 25℃to 50 during the addition.℃2.反应过程中或者降温有固体析出Solid was precipitate out after 1h reaction.℃The reaction mixture was cooled to -10, and solid was precipitate out.3.加料不溶解XX was added to the mixture, and the resulting suspension was stirred for 2h.4.加热溶解℃The suspension was heated to 90 and stirred until all solid was dissolved.5.反应变粘稠/变色The reaction mixture became sticky after 2hrs reaction/stirring.After 2hrs stirring, the mixture turned into black/brown/gray/yellow/red color.五、特殊结果叙述1.无进一步处理No further operation2.统一和其他批次一起后处理The work-up of this batch was together with the other batches that recorded in the following pages.3.检测条件，不需要后处理IPC check showed this condition is better/bad for this reaction. No further operation / screen reaction.Processs 组关于实验记录本内容方面的规范1. 反应时间要明确，统一规定为：XX(时): XX(分) 投料XX(时): XX(分) 检测XX(时): XX(分) 后处理XX(时): XX(分) 纯化及结果2. 反应必须有重要的反应现象叙述，包括物理现象和化学现象，比如放热，产生气体，产生沉淀，变粘稠，颜色变化等等。