反应详情

温度

70 °C

A stirred suspension of 3.69 g (19.7 mmol) 2-amino-6-phenyl-3H-pyrimidin-4-one in 4.5 ml (49.2 mmol) phosphorus oxychloride was heated at reflux for 2 h. The reaction mixture was then cooled to about 70° C. and poured cautiously onto 20 ml rapidly stirred ice-water. The mixture was briefly warmed to room temperature and then was recooled to 0° C. 100 ml 25% ammonium hydroxide solution was added and the resulting crystals were collected by filtration and washed with ice-cold water and then with a little ether to afford 3.49 g (86%) 4-chloro-6-phenyl-pyrimidin-2-ylamine as a pale yellow crystalline solid. EI-MS m/e (%): 207 (M{37Cl}+, 35), 206 ([M{37Cl}—H]+, 30)., 205 (M{35Cl}+, 100), 204 ([M{35Cl}—H]+, 56), 170 ([M—Cl]+, 35), 128 (([M—C6H5]+, 85).

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. temperatureThe mixture was briefly warmed to room temperature
4. customwas recooled to 0° C
5. filtrationthe resulting crystals were collected by filtration
6. washwashed with ice-cold water