HRID1607272
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
CONDITIONS
反应条件
- 温度
- 195 °C
PROCEDURE
实验过程
A mixture of 2-(p-methoxybenzoyl)-3-methyl-4-hydroxybenzofuran (2.0 gm; 7.0 mmoles), 99% hydrazine (50 mL) and potassium hydroxide (2.7 gm; 49 mmoles) in ethylene glycol (50 mL) was heated at 140° C. for a period of 2.5 hours and at 195° C. for one hour. The reaction mixture was cooled, poured in water, and extracted with ethylacetate. The organic phase was washed with 20% citric acid, with brine, dried (Na2SO4), and concentrated in vacuo. The residue was chromatographed on silica gel using 20% ethylacetate in hexane as eluent to yield 700 gm (37%) of 2-(p-methoxybenzyl)-3-methyl-4-hydroxybenzofuran, mp.130°-133° C.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- extractionextracted with ethylacetate
- washThe organic phase was washed with 20% citric acid, with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
- customThe residue was chromatographed on silica gel using 20% ethylacetate in hexane as eluent