HRID1742014
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Sodium hydride (1.44 g, 55% in oil, 0.033 mol) was washed with petrol 60°-80° and suspended in DMF (15 ml). To this the methyl (2-benzoylpyrrol-1-yl)acetate (4.0 g, 0.0165 mol) in DMF (15 ml) and methyl formate (20.3 ml, 0.33 mol) was added dropwise at room temperature. After 4 hours it was poured into 200 ml of 10% potassium carbonate, washed with diethyl ether (2×100 mls), then the aqueous was neutralised with concentrated hydrochloric acid and extracted with diethyl ether (2×100 ml). These extracts were washed with brine, dried and evaporated to give methyl 3-hydroxy-2- (2-benzoylpyrrol-1-yl)acrylate (3.86 g, 86%) as a white crystalline solid melting at 112°-113°.
WORKUP
后处理
- washwashed with diethyl ether (2×100 mls)
- extractionextracted with diethyl ether (2×100 ml)
- washThese extracts were washed with brine
- customdried
- customevaporated