HRID980462

反应详情

EQUATION

反应方程式

HRID 980462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionare added dropwise at room temperature
  2. customthe methanol is removed in vacuo
  3. dissolutionThe residue is dissolved in 10 ml of ethyl acetate, to the solution 2 ml of water
  4. additionare added
  5. customis adjusted to 2-3 with a 2N sodium hydrogen sulfate solution at 0° C
  6. customThe layers are separated
  7. customthe organic phase is dried
  8. filtrationfiltered
  9. distillationthe solvent is distilled off in vacuo