反应详情

温度

65 °C

A mixture of N-(2-chlorophenyl)-4,5-dihydropyrido[4,3-b]thieno[2,3-d]oxepine-2-carbohydrazonamide (42 mg, 0.11 mmol) from Example 230 and 92 mg (0.57 mmol) of N,N-carbonyldiimidazole in 3 ml of dimethylformamide was heated at 65° C. for 18 hours. The mixture was concentrated in vacuum and triturated with diethylether. The precipitate was collected, washed with ethyl ether and purified by flash chromatography eluting with 5% of methanol in methylene chloride to give 321 (14 mg, 31%). MS: (ESI+) 397.0

1. concentrationThe mixture was concentrated in vacuum
2. customtriturated with diethylether
3. customThe precipitate was collected
4. washwashed with ethyl ether
5. custompurified by flash chromatography
6. washeluting with 5% of methanol in methylene chloride