반응 #595303

반응 방정식

1-(trifluoromethyl)cyclopropanamine

diisopropylethylamine

succinic anhydride

→

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

용매

dioxane

반응 조건

후처리

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
   온도to cool to room temperature
5. 5
   농축the solution was concentrated
6. 6
   세척Repeatedly, the solution was washed alternately with ethyl acetate and with water
7. 7
   기타The combined organic phases were dried
8. 8
   농축concentrated

실험 절차

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.

출처