反应详情

A mixture of 200 mg (0.655 mmol) of 3-(2-amino-ethylamino)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine (water content: 0.48%), 72 mg (0.887 mmol) of potassium cyanate, 1.2 ml of ethanol, 1.2 ml of water and 46.8 ml (0.819 mmol) of acetic acid is stirred at RT for 15 hours. 2 ml of water are added to the resulting suspension and the mixture is filtered. Washing the filter residue with water and a small amount of ethanol and drying in vacuo (about 100 mbar, 8 hours, 1 00C) yield the title compound having a water content of 5.54%; m.p. 212-214° C.; ESI-MS: (M+H)+=347

1. filtrationthe mixture is filtered
2. washWashing the filter residue with water
3. dry with materiala small amount of ethanol and drying in vacuo (about 100 mbar, 8 hours, 1 00C)