HRID1534372
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationAfter filtering
- customthe mixture is evaporated in vacuo
- additionis added
- washthe mixture is washed with water
- customdried
- customevaporated
- customChromatography on silica gel Si60 in petroleum ether/ether=3:1 yields 730 mg (65% of theory) of glassy solid