反应 #595303

反应方程式

1-(trifluoromethyl)cyclopropanamine

diisopropylethylamine

succinic anhydride

→

4-oxo-4-{[1-(trifluoromethyl)cyclopropyl]amino}butanoic acid

溶剂

dioxane

反应条件

后处理

1. 1
   workup.WAITto stand overnight at this temperature
2. 2
   workup.STIRRINGAgain, stirring
3. 3
   workup.WAITwas continued for 20 min at 80° C.
4. 4
   温度to cool to room temperature
5. 5
   浓缩the solution was concentrated
6. 6
   洗涤Repeatedly, the solution was washed alternately with ethyl acetate and with water
7. 7
   其他The combined organic phases were dried
8. 8
   浓缩concentrated

实验过程

Slowly, 800.7 mg (4.96 mmol) of 1-(trifluoromethyl)cyclopropanamine and 0.85 ml (4.96 mmol) of diisopropylethylamine were added to a solution of 496 mg (4.96 mmol) of succinic anhydride in 10 ml of dioxane, with ice-cooling (10° C.). Stirring was continued for 20 min at room temperature, and the mixture was allowed to stand overnight at this temperature. Again, stirring was continued for 20 min at 80° C., the mixture was allowed to cool to room temperature, and the solution was concentrated. Repeatedly, the solution was washed alternately with ethyl acetate and with water. The combined organic phases were dried and concentrated. This gave 815.8 mg (73% of theory) of the desired compound.

来源