反应详情

7-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (2A) (1.03 g, 3.40 mmol) and N-(azepan-3-yl)-4-methylbenzenesulfonamide (6B) (1.00 g, 3.73 mmol) were dissolved in 2-methoxyethanol (30 ml) and triethylamine (2.4 ml), and the mixture was heated to 120° C. for 2 days. The solvents were evaporated and the crude product was dissolved in 100 ml of EtOAc and 100 ml of water. The aqueous phase was acidified with 1M potassium hydrogen sulphate until pH=2. The organic layer was separated and extracted with 50 ml of 1M aqueous potassium hydrogen sulphate, and 50 ml of brine, and dried over sodium sulphate. The solvent was evaporated and the crude product was purified by column chromatography on silica gel using EtOAc:heptane (1:1) as the eluent. Evaporation of the solvent gave compound (6C) as a white foam.

1. customThe solvents were evaporated
2. dissolutionthe crude product was dissolved in 100 ml of EtOAc
3. customThe organic layer was separated
4. extractionextracted with 50 ml of 1M aqueous potassium hydrogen sulphate, and 50 ml of brine
5. dry with materialdried over sodium sulphate
6. customThe solvent was evaporated
7. customthe crude product was purified by column chromatography on silica gel
8. customEvaporation of the solvent