HRID980462
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
12 g (55.75 millimoles) of 3-bromomethyl-benzoic acid are dissolved in 10 ml of anhydrous methanol and to the solution 22.30 ml of sodium methylate (concentration 5 millimoles/ml) are added dropwise at room temperature. The reaction mixture is stirred for 5-10 minutes, the methanol is removed in vacuo. The residue is dissolved in 10 ml of ethyl acetate, to the solution 2 ml of water are added and the pH of the mixture is adjusted to 2-3 with a 2N sodium hydrogen sulfate solution at 0° C. The layers are separated, the organic phase is dried, filtered and the solvent is distilled off in vacuo. Thus 8.55 g of the title compound are obtained, yield 92,3%.
WORKUP
后处理
- additionare added dropwise at room temperature
- customthe methanol is removed in vacuo
- dissolutionThe residue is dissolved in 10 ml of ethyl acetate, to the solution 2 ml of water
- additionare added
- customis adjusted to 2-3 with a 2N sodium hydrogen sulfate solution at 0° C
- customThe layers are separated
- customthe organic phase is dried
- filtrationfiltered
- distillationthe solvent is distilled off in vacuo