HRID1387906
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 mixture of 3-bromobenzaldehyde (10 g) and methoxy-carbonylmethylenetriphenylphosphine (20 g) was added toluene (150 ml), and the mixture was refluxed under nitrogen atmosphere for 2 hours. The solvent was evaporated, and the organic layer was washed with water and saturated sodium chloride solution, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column (ethyl acetate/hexane) to give methyl 3-bromocinnamate (10.7 g) as colorless crystals. 1H-NMR(δ ppm, CDCl3): 3.82 (3H, s), 6.44 (1H, d, J=16.0 Hz),
WORKUP
后处理
- temperaturethe mixture was refluxed under nitrogen atmosphere for 2 hours
- customThe solvent was evaporated
- washthe organic layer was washed with water and saturated sodium chloride solution
- dry with materialdried with anhydrous magnesium sulfate
- customUnder reduced pressure, the solvent was evaporated
- customthe residue was purified with silica gel column (ethyl acetate/hexane)