反应详情

Under a stream of argon, to compound (2) (8 g; 38 mmol), phosphorus oxychloride (72 mL) and phosphorus pentachloride (9.8 g; 47.6 mmol) were added in an ice bath. The resulting reaction mixture was stirred and refluxed for 8 hours, and excess phosphorus oxychloride was removed under reduced pressure. To the resulting reaction concentrate, ice water and concentrated aqueous ammonia were added and the resulting mixture was made alkaline to precipitate crude crystals. The crude crystals were separated by filtration and washed with water, and then dried under reduced pressure to give 6.1 g (yield: 75%) of the title compound (3).

1. customThe resulting reaction mixture
2. temperaturerefluxed for 8 hours
3. customexcess phosphorus oxychloride was removed under reduced pressure
4. customTo the resulting reaction
5. concentrationconcentrate
6. additionice water and concentrated aqueous ammonia were added
7. customto precipitate crude crystals
8. customThe crude crystals were separated by filtration
9. washwashed with water
10. customdried under reduced pressure