HRID649205

反应详情

EQUATION

反应方程式

HRID 649205 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixed solution of 0.55 g (0.005 mole) of 1-cyanomethylimidazole, 0.4 g (0.005 mole) of carbon disulfide and 10 ml of dimethyl sulfoxide was added 0.8 g (0.014 mole) of potassium hydroxide powder with stirring, and the reaction was carried out at room temperature for 1 hour. Then, 1.5 g (0.006 mole) of 1,2-dibromo-4-methylpentane was added dropwise with stirring, and the resulting solution was subjected to reaction for 2 hours. After completion of the reaction, 20 ml of water was added to the reaction solution, after which the resulting mixture was subjected to extraction with ethyl acetate, and the organic layer was washed with water and dried. The solvent was distilled off and the residue was purified by silica gel chromatography to obtain 0.45 g of the Z isomer and 0.3 g of the E isomer individually in the form of colorless crystals.

WORKUP

后处理

  1. stirringwith stirring
  2. customthe resulting solution was subjected to reaction for 2 hours
  3. additionwas added to the reaction solution
  4. extractionafter which the resulting mixture was subjected to extraction with ethyl acetate
  5. washthe organic layer was washed with water
  6. customdried
  7. distillationThe solvent was distilled off
  8. customthe residue was purified by silica gel chromatography
  9. customto obtain 0.45 g of the Z isomer and 0.3 g of the E isomer individually in the form of colorless crystals