有机合成英文实验历史纪录模板语句，献给写论文的你

potassiumsuperoxide (62 mg, 0.87 mmol, 4.5 equiv) and 18-crown-6-ether (23 mg, 0.087mmol, 0.45 equiv) in dry DMSO (0.5 mL).

6. 通过试管加料

To a stirred solution of compound 15 (8.61 g, 21.2 mmol) was added a solution of p-toluenesulfonicacid (6.0 g) in DCM via syringe over 5 min.

二、重排操作过程惯用说明了

1. 重排检测

After 1 h, TLC analysis (CH2Cl2/ hexane 3:1) showed the complete consumption of compound 15.

2. 放置过夜

The mixture was left standing overnight.

3. 苯基/甲苯带水

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 chloride as brown oil.

The aqueous portion was concentrated under reduced pressure followed by azeotropic removal of water with absolute EtOH.

4. 氢化重排

A mixture of compound 1 (190 g, 0.88mmol) and Raney Ni (20 g) in ethanol (1500 mL) and ethyl acetate (500 mL) was stirred under 1 atm at 25℃ for one hour.

5. 分水器

A mixture of TsOH.H2O (56.91 g, 0.3 mol) and toluene (400 mL) was heated to reflux to remove water by Dean-Stark trap.

6. 重排生成物

The reaction was exothermic.

7. 无线电波重排

The sealed vial was irradiated in the microwave on a Biotage Smith Synthesis at 150℃ for 10 mins.

三、后妥善处理操作过程惯用说明了

1. 过滤

The mixture was filtered through a Celite pad, and the filtrate was concentrated to give the crude product.

2. 淬灭

The reaction mixture was quenched by the addition of the saturated aqueous NH4Cl.

3. 碾碎

The residue was triturated with ether and filtered to afford a white solid.

4. 在两相当中连在一起

The residue was partitioned between ethyl acetate (100mL) and HCl (1 M aq., 50mL). The organic layer was washed with water, dried over 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.

5. 静止不动固化

The crude product was purified by prep-HPLC to give compound 4 as colorless thick oil, which was solidified on standing.

6. 在冻干机冻干

The white solid was re-crystallized from water, dried by hyophilization to give a white solid.

7. 提纯

1. 柱层析提纯

The crude product was chromatographed on silica gel (CH2Cl2 / MeOH 20:1→10:1→5:1) to give the compound 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.

2. 化学合成HPLC提纯

The crude product was purified by prep-HPLC to afford/give/yield desired product as a kind of white solid.

3. 化学合成TLC提纯

The crude product was purified by prep-TLC to afford/give/yield desired product as a kind of white solid.

4. 混合物

recrystallized from DCM/PE to give the desired product as a kind of white solid.

8. 转调pH

The pH was adjusted to around 9 by progressively adding solid NaHCO3

The mixture was adjusted to pH 9 with solid NaHCO3

9. 萃取

The aqueous layer was extracted with ethyl acetate (100mL × 4).

10. 浓缩

The mixture was evaporated to afford the crude product.

The mixture was concentrated to afford the crude product.

The solvent was removed to afford the crude product.

11. 湿

1. 湿

The organic layer was dried over MgSO4 and filtered the filtrate was concentrated under reduced pressure to give a redidue.

2. 真空湿

The precipitate was filtered and dried in vacuo (in/ undervacumm; under reduced pressure).

四、以外常见重排震荡描述

1. 加料生成物

A gentle reflux appeared through out the addition

Heat generated during the addition.

The temperature was increased from 25℃ to 50℃ during the addition.

2. 重排操作过程当中或者加温有固体分离出来

Solid was precipitate out after 1h reaction.

The reaction mixture was cooled to -10℃, and solid was precipitate out.

3. 加料不分解

XX was added to the mixture, and the resulting suspension was stirred for 2hrs.

4. 加热分解

The suspension was heated to 90℃ and stirred until all solid was dissolved.

5. 重排不定粉末状/不定色

The reaction mixture became sticky after 2hrs reaction/stirring.

After 2hrs stirring, the mixture turned into black/brown/gray/yellow/red.

五、特殊结果叙述

1. 无全面性妥善处理/提纯

No further operation/purification.

2. 统合和其他5台一起后妥善处理

The work-up of this batch was together with the other batches that recorded in the following pages.

3. 检测条件，不需要后妥善处理

IPC check showed this condition is better/bad for this reaction. No further operation for condition screen reaction.

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