반응 #84215

반응 방정식

3-hydroxy-4-(difluoromethoxy)-benzoic acid methyl ester

K2CO3

NaI

bromo-methylcyclopropane

→

3-(cyclopropylmethoxy)-4-(difluoromethoxy)-benzoic acid methyl ester

용매

water

DMF

반응 조건

후처리

1. 1
   온도The suspension was cooled to room temperature
2. 2
   workup.STIRRINGunder stirring
3. 3
   온도The heterogeneous mixture was cooled to 0 to 5° C. for 60 to 90 minutes
4. 4
   여과the solid filtered on a gooch funnel
5. 5
   세척washed with water (50 ml)
6. 6
   기타An orange solid was obtained
7. 7
   기타It was dried under vacuum at room temperature

실험 절차

3-hydroxy-4-(difluoromethoxy)-benzoic acid methyl ester (5 g, 22.9 mmol), K2CO3 (4.75 g, 34.4 mmol), NaI (0.34 g, 2.3 mmol) and bromo-methylcyclopropane (3.7 g, 27.5 mmol) were dissolved in DMF (25 ml), and the heterogeneous mixture was stirred and warmed at 80° C. for two hours. The suspension was cooled to room temperature, and water (50 ml) was added under stirring. The heterogeneous mixture was cooled to 0 to 5° C. for 60 to 90 minutes, and the solid filtered on a gooch funnel and washed with water (50 ml). An orange solid was obtained. It was dried under vacuum at room temperature. (yield 95.8%).

출처