这个你可以甩两眼.docx

这个你可以甩两眼！ Enote操作中可用英文例句反应部分sealed tube 封管pressure tank reactor 高压釜freshly prepared 新制的The suspension 悬浮液added in several portion分批加ssaturated aqueous NaHCO3 饱和NaHCO3水溶液Grignard Reagents 格氏试剂initiated by引发Into a 200 ml 4-necked roundbottom flask purged and maintained with an inert atmosphere of nitrogen,在充满氮气的200 毫升四颈圆底烧瓶中A 200 ml flask was charged with a solution of SM in THF under nitrogen atmosphere,在充满氮气的200 毫升烧瓶中加入SM的THF溶液XX was added via microsyringe to.用微量注射器把XX加入到The flask was evacuated and flushed three times with nitrogen, followed by flushing with hydrogen. The mixture was stirred 2h at room temperature under an atmosphere of hydrogen (balloon).反应瓶用氮气置换三次，紧接着通氢气。在氢气环境下（氢气球），室温下混合搅拌2个小时。This was followed by the addition of a solution of SM (50 g) in H2O (50 ml), which was added dropwise with stirring at 0 degrees C in 15 mins.将50 g SM溶于50mL水制成的溶液在0条件下滴加到上述混合液中，滴加时间为15分钟。This solution was slowly transferred to a solution of XXX in anhydrous THF (20 mL).该溶液被慢慢转移到XXX的THF(20 mL)溶液中To the above H2(g) was introduced in在以上混合液中通入H2气The above mixture was stirred for 1 hour at -20 degrees C.以上混合物在-20度搅拌1小时The final reaction mixture was irradiated with microwave radiation for 10 mins at 90 degrees C.最终的混合物用微波辐射10分钟在90The reaction mixture was then heated to reflux for 30min反应液加热回流30 分钟The temperature was increased to room temperature naturally.自然升温到室温The reaction mixture was sonicated at room temperature for 3h.反应混合物在室温下超声3h。The mixture was heated for 1.5 hr under reflux and water separation.混合物在水分离的条件下回流1.5h。The water formed in the reaction was removed via a Dean-Stark tube反应中形成的水份通过Dean-Stark管除去。The temperature of the external bath was carefully maintained between -20 and -25 degrees C during the addition.外面冰水浴的温度要保持在-20 -25之间。Ozone was bubbled slowly into the solution until the reaction mixture turned colorless; Nitrogen was then passed through the solution to remove any excess ozone.臭氧被慢慢地鼓泡进入反应液直到反应液变成无色，然后通入氮气来去除多余的臭氧After cooled to room temperature, the reaction mixture was 冷却到室温后，反应混合物被The reaction was cooled to -20 degrees C.该反应冷却到-20The resulting solution was kept undisturbed overnight生成的溶液被静置过夜后处理部分The reaction mixture was poured into 200g of crushed ice. The isolated solid was collected and purified by recrystalization with ethanol.该反应混合物加入到200 g碎冰中碎灭。析出的固体被收集，并用乙醇重结晶纯化。The reaction was then quenched by the addition of 300 mL of water.该反应加入300 mL的水进行淬灭。The reaction mixture was cooled to room temperature该反应混合物被冷却至室温。The resulting solution was diluted with 50 ml of water, then extracted with .最终的反应液加入50 ml的水进行稀释，然后萃取用.The residue was diluted with water, then adjusted to pH 67 with sodium bicarbonate. The solid was collected by filtration.反应液加水稀释，用碳酸氢钠调pH值到67，过滤收集生成的固体。The solid was filtered out. The filtrate was concentrated under vacuum.固体被过滤掉。滤液在真空状态下浓缩。The pH value of the solution was adjusted to 67 with NaHCO3.用碳酸氢钠将溶液的pH值调到67。The product was precipitated by the addition of NH3H2O.该产品加入氨水，使其沉淀。The mixture was filtered through a Celite pad该混合物被过滤通过矽藻土垫。The resulting mixture was washed with 2x500 mL of saturated brine得到的混合物用2x500 mL的饱和食盐水洗涤。The resulting solution was extracted with 3x40 mL of ethyl acetate. The organic layers were combined, washed with sodium carbonate (aq.) and brine, dried and concentrated under vacuum. The residue was applied on a silica gel column and eluted with ethyl acetate/hexane (1/20) to give 1.5g product as a colorless solid.反应溶液用3x40 mL乙酸乙酯提取。将有机层合并，用碳酸钠（aq.）和盐水洗涤，干燥，在真空状态下浓缩。得到的粗品，过硅胶柱，用乙酸乙酯/正己烷（1 / 20）洗脱，得到1.5g无色固体产品。The reaction mixture was partitioned between CH2Cl2 and water. The aqueous layer was extracted again with CH2Cl2.The combined organic layer was dried over anhydrous sodium sulfate and concentrated under vacuum.反应混合物在二氯甲烷和水中分层。水层用二氯甲烷萃取。将合并的有机相用无水硫酸钠干燥，在真空状态下浓缩。The mixture was poured into 20 mL of water and 20 mL of ethyl acetate.该混合物加入到20 mL的水和20 mL乙酸乙酯。The organic phase was separated,有机相被分离The mixture was dried over anhydrous magnesium sulfate该混合物用无水硫酸镁干燥The solid was dried in an oven under reduced pressure固体在真空干燥箱里干燥The combined aqueous layer was dried by lyophilization.合并的水相冻干干燥。The solid was dried in an oven under reduced pressure.固体在真空干燥箱被干燥The solid was dried under vacuum.固体在真空状态下被干燥The solid was dried under infrared light.固体在红外光下干燥The solid was air-dried.固体被风干The solvent was evaporated in vacuo to give yellow syrup.在真空中蒸发溶剂得到黄色的油状物。The solvent was removed under reduced pressure溶剂在减压的条件下被分离The solvent was removed by distillation under vacuum.减压蒸出溶剂The resulting solution was decolorized by the addition of active carbon.最终的溶液加入活性炭脱色。The residue was purified by thin layer chromatography developed with ethyl acetate/hexane (1/20).残留物用乙酸乙酯/正己烷（1 / 20）的薄层色谱法进行纯化。The dried solid was triturated with hot acetone (3x20mL) and filtered to remove inorganic salts.干燥的固体放在研钵里加热丙酮（20mL）研磨，重复三次，过滤除去无机盐。chromatography board 层析板The residue was purified by preparative TLC (EtOAc:n-hexane = 1:1).残余物经制备薄层色谱法（乙酸乙酯：正己烷= 1:1）进行纯化。The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:30).残留物被纯化用乙酸乙酯/石油醚（1:30）的硅胶柱。The mixture was neutralized with Dowex 50WX8-200 ion-exchange resin.混合物通过Dowex 50WX8-200离子交换树脂被中和。The crude product was re-crystallized from EtOAc/PE in the ratio of 1:2.粗产品用乙酸乙酯和石油醚比例为1:2经行重结晶。The crude product was re-crystallized from ethyl acetate/petroleum ether in the ratio of 1:2.粗品用乙酸乙酯：石油醚比例为1:2进行重结晶。The product was collected from reaction mixture by steam distillation.该产品采用水蒸气蒸馏法从反应混合物中收集。The crude product was purified by distillation under reduced pressure (76 mm Hg) and the fraction was collected at 68-70 degrees C.粗产品被纯化通过减压蒸馏（76毫米汞柱），并收集68-70的馏分。性状：syrup，foam, crystalline, sticky gum, semi-solid糖浆，泡沫，晶体，粘稠物，半固体结论部分成功但没有结果的原因：which was used in the next step without further purification.粗品没经过进一步的纯化直接用于下一步The product was used in the next step directly without further purification.粗品没经过进一步的纯化直接用于下一步It was difficult to purify.产物很难纯化TLC showed no starting material.TLC检测表明已没有开始原料The reaction was successful and confirmed by TLC.TLC确定反应是成功的The product has very good water-solubility. Only small amount of product was extracted from the aqueous layer.产物有很好的水溶性，仅有少量产物从水相中萃取出来失败的原因：The reaction did not happen.该反应没有发生。The starting material was not transformed completely and it was difficult to separate it from the reaction mixture.原料没有完全反应，很难从反应混合物中分离出来The reaction did not go to completion. The S.M was hard to separate from the target product.反应没有完全。初始原料很难从目标产品中分离。After stirred for 3h, TLC showed the SM did not transform to product any further.搅拌3小时后，TLC检测发现初始原料没有