反应详情

A mixture of 200 mg (0.5 mmol) crude (3-chloro-4-fluoro-phenyl)-[6-(4-chloromethyl-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-amine in 15 ml absolute ethanol is treated with 0.8 ml (5 mmol) of a 33% solution of dimethylamine in ethanol (Fluka, Buchs, Switzerland) and then heated under reflux for 1 h. The almost clear solution is cooled and the solvent evaporated. The residue is dissolved in a mixture of dichloromethane and ethanol (95:5), washed with water, dried over sodium sulfate and the solvent evaporated. Purification of the crude material through flash chromatography using first dichloromethane/ethanol 95:5 plus 1% conc. ammonia and then dichloromethane/ethanol 9:1 plus 1% conc. ammonia gives the title compound; m.p. 274-276° C.; MS-ES+: (M+H)+=396.

1. temperatureheated
2. temperatureunder reflux for 1 h
3. temperatureThe almost clear solution is cooled
4. customthe solvent evaporated
5. dissolutionThe residue is dissolved in a mixture of dichloromethane and ethanol (95:5)
6. washwashed with water
7. dry with materialdried over sodium sulfate
8. customthe solvent evaporated
9. customPurification of the crude material through flash chromatography