反应详情

Under a stream of argon, to compound (5) (4.26 g; 17.4 mmol), phosphorus oxy-chloride (39 mL) and phosphorus pentachloride (4.48 g; 21.8 mmol) were added in an ice bath. The resulting reaction mixture was stirred and refluxed for 7 hours, and then evaporated under reduced pressure to remove phosphorus oxychloride. To the resulting residue, ice water and concentrated aqueous ammonia were added and the resulting reaction mixture was made alkaline. The solids which precipitated out were separated by filtration and washed with water, and then dried under reduced pressure to give 4.06 g (yield: 94%) of the title compound (6).

1. customThe resulting reaction mixture
2. temperaturerefluxed for 7 hours
3. customevaporated under reduced pressure
4. customto remove phosphorus oxychloride
5. additionTo the resulting residue, ice water and concentrated aqueous ammonia were added
6. customthe resulting reaction mixture
7. customThe solids which precipitated out
8. customwere separated by filtration
9. washwashed with water
10. customdried under reduced pressure