HRID1872365
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
- 70 °C
PROCEDURE
实验过程
To a mixture of dimethylmalonate (4 ml), 2-hydroxy-4-octyloxybenzaldehyde (2.50 g) and piperidine (0.1 ml) in methanol (10 ml) was added acetic acid (0.01 ml), and the mixture was stirred for 3 hours at 70° C. The solvents were removed under reduced pressure, and the residue was dissolved in ethyl acetate, and washed with 0.5N hydrochloric acid, water and brine, and dried over magnesium sulfate. The magnesium sulfate was filtered off, and filtrate was evaporated under reduced pressure, and the precipitate was collected by filtration, and washed with n-hexane, and dried to give Methyl 7-octyloxycoumarin-3-carboxylate (0.94 g).
WORKUP
后处理
- customThe solvents were removed under reduced pressure
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with 0.5N hydrochloric acid, water and brine
- dry with materialdried over magnesium sulfate
- filtrationThe magnesium sulfate was filtered off
- customfiltrate was evaporated under reduced pressure
- filtrationthe precipitate was collected by filtration
- washwashed with n-hexane
- customdried