反应 #166048

反应方程式

acetic anhydride

Tranexamic acid

sulfuric acid

acetic anhydride

water

→

trans-{4-[(acetylamino) methyl]cyclohexyl}carboxylic acid

收率 98.0%

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 1 hour
2. 2
   浓缩The reaction solution was concentrated under reduced pressure
3. 3
   其他the residue was further azeotroped with toluene
4. 4
   其他The resulting precipitates
5. 5
   过滤were collected by filtration
6. 6
   洗涤washed with ether
7. 7
   其他dried under reduced pressure

实验过程

Tranexamic acid (10 g, 63.6 mmol) was suspended in acetic anhydride (50 mL), this suspension was added with concentrated sulfuric acid (0.01 mL) at room temperature, and the mixture was stirred overnight at the same temperature. Under ice cooling, the reaction mixture was added with water (100 mL), and the mixture was stirred at room temperature for 1 hour to decompose excess acetic anhydride. The reaction solution was concentrated under reduced pressure, and the residue was further azeotroped with toluene. The resulting precipitates were collected by filtration, washed with ether, and dried under reduced pressure to obtain trans-{4-[(acetylamino) methyl]cyclohexyl}carboxylic acid as white solid (12.46 g, 98%).

来源