Phosphorus oxychloride → 2-Chloro-1,10-phenanthroline

HRID 241393

반응식

HRID 241393 반응식
C[N:2]1[C:15]2[C:6](=[CH:7][CH:8]=[C:9]3[C:14]=2[N:13]=[CH:12][CH:11]=[CH:10]3)[CH:5]=[CH:4][C:3]1=O.P(Cl)(Cl)([Cl:19])=O.P(Cl)(Cl)(Cl)(Cl)Cl>>[Cl:19][C:3]1[CH:4]=[CH:5][C:6]2[C:15](=[C:14]3[C:9](=[CH:8][CH:7]=2)[CH:10]=[CH:11][CH:12]=[N:13]3)[N:2]=1

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 35813871-Methyl-1,10-phenanthrolin-2(1H)-one

생성물 1

HCID 3551932-Chloro-1,10-phenanthroline수율 75%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-abc0e3193ca04d4bb617865837a2020f
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648194B2

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