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

HRID 716553

反応式

HRID 716553 の反応式
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

参加物

4

反応物 3

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

生成物 1

HCID 3551932-Chloro-1,10-phenanthroline収率 75%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cbdf28e7d2ab48edafa77d6f502aa9d8
出典データセット
uspto-grants-2015_11
特許番号
US09187690B2

関連ノート

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