HRID380737
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
1.46 g (5.5 mmol) of 3-(4-ethoxytetrahydrofuran-3-yloxy)-4-methoxybenzonitrile (A7) and 3.0 g (55.0 mmol) of potassium hydroxide are heated at 140° C. for 3 h in 15 ml of glycerol. The mixture is treated with 50 ml of water, washed with 2×25 ml of ethyl acetate and the aqueous phase is acidified by dropwise addition of 30 ml of 2 N hydrochloric acid with ice-cooling. The mixture is subsequently stirred for 1 h, filtered and the precipitate is washed with ice water. 1.49 g of the title compound of m.p. 135-138° C. are obtained.
WORKUP
后处理
- washwashed with 2×25 ml of ethyl acetate
- additionthe aqueous phase is acidified by dropwise addition of 30 ml of 2 N hydrochloric acid with ice-
- temperaturecooling
- filtrationfiltered
- washthe precipitate is washed with ice water