反应详情

温度

60 °C

42.4 ml (0.44 mole) of phosphorus oxychloride were added to a stirred and ice-cooled solution of 81.2 g (0.4 mole) of compound IV in 160 ml of pyridine. The temperature reached 45° C. Thereupon the mixture was heated to 60° C. The reddish-brown oil obtained was poored immediately in 1 kg of an ice-water mixture with stirring. The precipitate was filtered, washed with ice-cold water and dried. The crude product obtained was crystallized from pyridine (1.5 ml/g) and water (9 mg/g). Melting point: 162° C. Yield: 61% (452 g).

1. customreached 45° C
2. customThe reddish-brown oil obtained
3. stirringwith stirring
4. filtrationThe precipitate was filtered
5. washwashed with ice-cold water
6. customdried