反应详情

A mixture of (2E)-1-{6-[(3-cyclobutyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)oxy]-3-pyridinyl}-3-(dimethylamino)-2-propen-1-one (D53) (195 mg, 0.5 mmol) and hydrazine hydrate (0.4 ml) in methanol (3 ml) was heated at reflux for 24 hours. The reaction mixture was cooled and applied to a SCX ion exchange cartridge (Varian bond-elute, 10 g) and washed with methanol and then a mixture of 0.880 ammonia/methanol (1:9). The combined basic fractions were concentrated in vacuo and the resulting residue purified by column chromatography eluting with a mixture of 0.880 ammonia:methanol:dichloromethane (1:9:90) to afford the title compound (E215). MS (ES+) m/e 361 [M+H]+.

1. temperaturewas heated
2. temperatureat reflux for 24 hours
3. temperatureThe reaction mixture was cooled
4. washwashed with methanol
5. additiona mixture of 0.880 ammonia/methanol (1:9)
6. concentrationThe combined basic fractions were concentrated in vacuo
7. customthe resulting residue purified by column chromatography
8. washeluting with a mixture of 0.880 ammonia:methanol:dichloromethane (1:9:90)