HRID1059301

反应详情

EQUATION

反应方程式

HRID 1059301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

30.2 g of cis-1,2,3,6-tetrahydrophthalimide was dissolved in 200 ml of N,N-dimethylformamide. After adding 38.7 g of potassium carbonate and 30.4 g of benzyl chloride, the resulting mixture was stirred at 50° C. for 3 hours and further at room temperature overnight. Then the reaction mixture was diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate. The organic layer was washed successively with water and a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. After filtering, the solvent was distilled off under reduced pressure. The crude crystals thus obtained were ground and washed with diisopropyl ether and n-hexane followed by filtration. Thus 39.1 g of the title compound was obtained as pale yellow crystals.

WORKUP

后处理

  1. washwashed with water
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. washThe organic layer was washed successively with water
  4. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate
  5. filtrationAfter filtering
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe crude crystals thus obtained
  8. washwashed with diisopropyl ether and n-hexane
  9. filtrationfollowed by filtration