HRID1461654

反应详情

EQUATION

反应方程式

HRID 1461654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

22.6 g (0.1 mol) of 1-(3-chloro-α,α-dimethylbenzylamino)-2-propanone prepared by the method of Reference Example 5, was dissolved in 200 ml of acetone, and 14.0 g (0.11 mol) of potassium carbonate was added thereto. The mixture was cooled with ice water, and then 15.5 g (0.1 mol) of phenylacetyl chloride was gradually dropwise added thereto under stirring. After completion of the dropwise addition, the reaction mixture was returned to room temperature and stirred for 3 hours. Then, the solvent was distilled off under reduced pressure, and then water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was crystallized from n-hexane to obtain 21.5 g (yield: 62.5%) of the desired compound.

WORKUP

后处理

  1. additionAfter completion of the dropwise addition
  2. customwas returned to room temperature
  3. stirringstirred for 3 hours
  4. distillationThen, the solvent was distilled off under reduced pressure
  5. additionwater was added to the residue
  6. extractionthe mixture was extracted with ethyl acetate
  7. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe residue was crystallized from n-hexane