HRID1534372

反应详情

EQUATION

反应方程式

HRID 1534372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.1 g (3.0 mmol) of the compound from Example 95 in 10 ml of dimethylformamide, 2.2 ml (15.3 mmol) of 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene and 0.65 g of copper(I) oxide are stirred at 80° C. for 12 h in an argon atmosphere. After filtering, the mixture is evaporated in vacuo, the residue is taken up with methylene chloride, 1N aqueous hydrochloric acid is added, then the mixture is washed with water, dried and evaporated. Chromatography on silica gel Si60 in petroleum ether/ether=3:1 yields 730 mg (65% of theory) of glassy solid.

WORKUP

后处理

  1. filtrationAfter filtering
  2. customthe mixture is evaporated in vacuo
  3. additionis added
  4. washthe mixture is washed with water
  5. customdried
  6. customevaporated
  7. customChromatography on silica gel Si60 in petroleum ether/ether=3:1 yields 730 mg (65% of theory) of glassy solid