HRID978115
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
To a solution of ethyl 4-hydroxy-3-methylbenzofuran-2-carboxylate (220 mg, 1 mmol) in dichloroethane (10 ml) was added aluminum chloride (665 mg, 5 mmol). To the resulting brown solution was added acetyl chloride (0.178 ml, 2.5 mmol). The mixture was stirred for 5 hours at room temperature. Ice and water (20 ml) was added. The mixture was extracted with ethyl acetate. The extracts were dried and concentrated to a white solid which was then treated with 1 ml of 10% K2CO3 aqueous solution in 10 ml methanol for 2 hours. The resulting mixture was poured into 0.1N HCl (25 ml) and filtered. The solid obtained was recrystallized from ethyl acetate/toluene to give the title compound (130 mg, 50%).
WORKUP
后处理
- extractionThe mixture was extracted with ethyl acetate
- customThe extracts were dried
- concentrationconcentrated to a white solid which
- additionwas then treated with 1 ml of 10% K2CO3 aqueous solution in 10 ml methanol for 2 hours
- additionThe resulting mixture was poured into 0.1N HCl (25 ml)
- filtrationfiltered
- customThe solid obtained
- customwas recrystallized from ethyl acetate/toluene