订购/客服热线:137-9521-9287
当前位置:首页 » 珂臻学苑

实验记录常用英文表达句型

发布时间:2016-10-23

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
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
1
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 CH 2 Cl 2 (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 CH 2 Cl 2 (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 H 2 O (378 ul)
分批加入 in portions/portionwise
一次性加入 in one portion
滴加 dropwise
2.催化量的
Et 3 N (20 mL, 142 mmol) and a catalytic amount of DMAP were added the solution of
compound 1 (4.549 g, 46.4 mmol) in CH 2 Cl 2 (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 CH 2 Cl 2 (5 ml) until it turned light blue. The
solution was purged with argon at -78 for 10 min to remove the excess O ℃
3 .
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).
2
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 CH 2 Cl 2 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 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
reflux) for 2 hrs (or overnight)
2. 反应检测
a. After 1 h, TLC analysis (CH 2 Cl 2 / 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 . ℃
3
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 2 O (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 .
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 dropwise Br (3.45 g, 22
mmol) in CH
2
2 Cl 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.
4
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 NH 4 Cl.
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 (MgSO 4 ) 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 solidfied 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 (CH 2 Cl 2 / MeOH
20:1→10:1→5:1) to give the compond 8 (0.282 g, 51%) as a white solid.
5
The crude product was purified by column chromatography on silica gel eluted with
(CH 2 Cl 2 / 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/yield
7.3 制备 TLC 纯化
Be purified by prepare TLC to afford/give/yield
7.4 重结晶
Recrystallized from
8.调 PH
The pH was adjusted to around 9 by progressively adding solid NaHCO 3 .
The mixture was adjusted to pH 9 with solid NaHCO 3 .
酸化: be acidified to 碱化: be basified to 中和: be neutralized
9.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.
4
MgSO
11.2 真空干燥
The precipitate was filtered and dried (in/under vacumm; under reduced pressure).
6
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 operation
2. 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.
7
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。
3. 加料过程必须详细,如加料时的温度,及加料过程中的温度变化等,是否滴
加(dropwise), 快速加(quickly),还是分批加(in portions);滴加的话,写清
楚大概的滴加时间。
4. 反应必须有应有的检测,并必须写明是用什么检测(TLC,HPLC,LC-MS 等)
TLC 的话,要在右下角划上 TLC 图,图上应如实反应你的点板情况,一般包含
3 个点,反应原料点,反应液点和二者的混合点;同时,TLC 还请标明展开剂及
配比
HPLC 或 LC-MC 等检测请简要描述检测结果,如反应基本完全,或者原料和产
物比例 X%: X%等等。
5. 反应后处理必须有详细叙述(摸索条件不做后处理的例外),包括用什么萃取,
萃取量,萃取次数(以上均可以为概数),后处理中调整酸碱度的需注明用什么
试剂,试剂的状态(饱和的,X%浓度的等等),调整后的 pH 值,调整过程中需
要注意事项(如,是否滴加调到 pH 9,是否搅拌情况下调整 pH 值,等等)
6. 反应的纯化过程必须详细(无纯化的除外),必须写明。
7. 反应必须有反应结果和反应目的。一个失败的反应必须阐明原因,摸索条件
的反应必须写明改反应是测试条件,不需要后处理或者纯化,而且,必须写明通
过检测条件是否可行,或者同时开展的几个摸索条件的反应可以横向进行比较,
哪个条件为最优等,一个完整的反应结果包括理论产量,实际产量,产率,相关
标准品谱图信息(核磁直接用核磁谱图的完整标题记录谱图信息,HPLC 或者
MC 需要在前面标明是 HPLC 还是 MS),实验记录者签名,实验记录结束日期。
8
Notebook 记录注意事项:
1. 记录一定要准确,详实。不要漏记任何信息。比如:展开剂,洗脱液及其比
例;后处理;重结晶试剂的量等。做到能够被重复。
2. 对于 Sourse; M. W; W.T; Mole (eq.)必须写全,如果某试剂有危险需要戴
防毒面具等,需要在 Note 中写明。对于 Source, 如果是中间体,写出它的 batch
NO;如果是原料,国产的,写 domestic;如果是进口试剂,写出公司名称和试剂
ID 号,如 Aidrich 163767
3. 谱图编号要写出。在记录的时候,在过程中如果打谱了,不论结果如何,都
要写出编号,且用括号括起来。公司的记录本则在相应的位置写出。
4. TLC 版的图示可在各页右侧标出。最好用尺子画,便于整条美观。公司的记
录本则在相应的位置写出。
5. 一个实验完成后,在接下来的记录页上的空白处画一斜线(/)。
6. 如果一个实验今天没做完,在记录的右侧写上日期和姓名,在下一行画一横
线,第二天接着做后处理等再记录的时候,在左边写上日期(见实例所示)。
7. 记录本应每天拿给组长或指定人员审阅一次。
8. 记录本必须当天记录。
9. 如果一个实验没有在接下来的一页上书写,而在其他页上继续写的时候,在
此页写末尾写上“Continued to page”。
10. 所有的反应均应有相关记录不论反应成功与否。反应数的统计以实验记录为
准。
11. 对于一些非标准的缩写,可以一直写全称,也可以在第一次写的时候在括号
内注明全称,然后在目录页中专门来标明这些缩写。鉴于很多同事反映目录页不
够用,所以建议写全称。
12. 对于一个能被解释的反应写明失败,描述必须事实地,客观地,并且有数据
支持的,如果不再继续此反应,必须说明原因;如果某反应不能达到预期的结果,
必须客观地描述结果。
9