反応 #80283

反応方程式

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

dimethylamine

water

→

desired compound

収率 60.0%

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

収率 60.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度under cooling with ice
2. 2
   抽出extracted with dichloromethane
3. 3
   洗浄The organic layer was washed with water
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   その他The oily substance obtained by concentration under reduced pressure
6. 6
   その他was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1)

実験手順

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.

出典