反应详情

A mixture of the product of Stage (ii) (1.8 g), paraformaldehyde (0.3 g) and dimethylamine hydrochloride (0.75 g) in acetic acid (14 ml) was heated at 80°-100° under nitrogen for 2 h. The reaction mixture was cooled (20°), evaporated in vacuo and purified by flash chromatography (L) to give a foam. A sample (0.2 g) was stirred in 0.88 ammonia 10 ml) for 3 days to precipitate to title compound (100 mg) as a solid. m.p. 171°-173° (foams).

1. temperaturewas heated at 80°-100° under nitrogen for 2 h
2. temperatureThe reaction mixture was cooled (20°)
3. customevaporated in vacuo
4. custompurified by flash chromatography (L)
5. customto give a foam
6. customto precipitate to title compound (100 mg) as a solid