反应详情

The operation is carried out as in Stage 1 of Example 10 starting from 280 mg of the product obtained in Stage 1 of Example 7, 4 ml of methylene chloride, 0.2 ml of triethylamine and 255 mg of 4-chlorobenzenesulphonic acid chloride in place of the 4-methyl-benzenesulphonic acid chloride then the reaction medium is agitated at ambient temperature for 30 minutes. Then 2 ml of water is added, followed by extracting with 3×5 ml of methylene chloride, washing with 5 ml of saturated sodium chloride, drying, evaporating, impasting in 5 ml of ether then in 5 ml of pentane, separating, and drying. After chromatography on silica eluting with methylene chloride/CH3CN in a proportion of 70/30, 350 mg of expected product is obtained in the form of a beige solid.

1. extractionby extracting with 3×5 ml of methylene chloride
2. washwashing with 5 ml of saturated sodium chloride
3. customdrying
4. customevaporating
5. customin 5 ml of pentane, separating
6. customdrying