반응 #80283

반응 방정식

4-allyloxycarbonyl-5-(4,6-dimethoxypyrimidin-2-yl)oxy-2-methylbenzofuran-3-carbonyl chloride

dimethylamine

water

→

desired compound

수율 60.0%

Allyl 5-(4,6-Dimethoxypyrimidin-2-yl)oxy-3-dimethylcarbamoyl-2-methylbenzofuran-4-carboxylate

수율 60.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도under cooling with ice
2. 2
   추출extracted with dichloromethane
3. 3
   세척The organic layer was washed with water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타The oily substance obtained by concentration under reduced pressure
6. 6
   기타was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1)

실험 절차

3.0 g of 4-allyloxycarbonyl-5-(4,6-dimethoxypyrimidin-2-yl)oxy-2-methylbenzofuran-3-carbonyl chloride was dissolved in 13 ml of dichloromethane, and 1.5 g of a 50% dimethylamine aqueous solution was dropwise added thereto under cooling with ice. After stirring for 30 minutes, the reaction solution was poured into water and extracted with dichloromethane. The organic layer was washed with water and then dried over anhydrous sodium sulfate. The oily substance obtained by concentration under reduced pressure, was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1) to obtain 1.84 g (yield: 60%) of the desired compound.

출처