تفاعل #80283

معادلة التفاعل

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

dimethylamine

water

→

desired compound

المردود 60.0%

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

المردود 60.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder cooling with ice
2. 2
   استخلاصextracted with dichloromethane
3. 3
   غسيلThe organic layer was washed with water
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىThe oily substance obtained by concentration under reduced pressure
6. 6
   أخرىwas purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1)

الإجراء التجريبي

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.

المصدر