反应详情

温度

60 °C

Phosphorus oxychloride (POCl3) (42.4 ml - 0.44 mole) was added to a stirred and ice-cooled solution of IV (81.2 g - 0.4 mole) in pyridine (160 ml). The temperature reached 45° C. After this addition, the mixture was heated to 60° C. The reddish-brown oil was poured immediately in 1 kg of ice/water with stirring. The precipitate was filtered, washed with ice-cold water, and dried. The crude product was crystallized from pyridine (1.5 ml/g) and water (9 ml/g).

1. customreached 45° C
2. additionAfter this addition
3. stirringwith stirring
4. filtrationThe precipitate was filtered
5. washwashed with ice-cold water
6. customdried
7. customThe crude product was crystallized from pyridine (1.5 ml/g) and water (9 ml/g)