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PH
9.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北京的长城
1.加料放热封顶条幅
2.反应过程中或者降温有固体析出
3.加料不溶解
春节古诗词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
公主的画法一、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 (dropwi / 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/portionwi
一次性加入 in one portion
滴加 dropwi
2.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 dropwi 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 O
5.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 dropwi (via addition funnel or syringe) to the above mixture at 10 ℃
(while maintaining gentle reflux;
℃.
while keeping internal temperature between 10 ℃ - 30)
唐朝名将
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 and
then 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 (or
overnight)
d.The reaction mixture (solution or suspension) was allowed to reflux (or heat to
纺的成语
reflux) 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
龙湖森林公园
The aled vial was irradiated in the microwave on a Biotage Smith Synthesis at 150 for 10 min.℃
9. 抽真空
The mixture was degasd for 10 min and refilled with N .
2
10. 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 dropwi 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 parator funnel and parated.
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 parated.
6. 静止固化
The crude product was purified by prep-HPLC to give compound 4 as colorless thick oil, which was solidfied on standing.
笔筒设计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.
