Hydrogen Peroxide → Tris(2-bromo-6-pyridyl)phosphine oxide

HRID 13634

反応式

HRID 13634 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([P:8]([C:16]2[N:21]=[C:20]([Br:22])[CH:19]=[CH:18][CH:17]=2)[C:9]2[N:14]=[C:13]([Br:15])[CH:12]=[CH:11][CH:10]=2)[N:3]=1.[OH:23]O.O>C(Cl)(Cl)Cl>[Br:22][C:20]1[CH:19]=[CH:18][CH:17]=[C:16]([P:8](=[O:23])([C:9]2[N:14]=[C:13]([Br:15])[CH:12]=[CH:11][CH:10]=2)[C:4]2[N:3]=[C:2]([Br:1])[CH:7]=[CH:6][CH:5]=2)[N:21]=1

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 15190498Tris(2-bromo-6-pyridyl)phosphine

生成物 1

HCID 21708779Tris(2-bromo-6-pyridyl)phosphine oxide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A suspension, heated to boiling, of 50.2 g (100.0 mmol) of tris(2-bromo-6-pyridyl)phosphine in 500 ml of chloroform was admixed with intensive stirring dropwise with a mixture of 11 ml of 35% by weight H2O2 and 50 ml of water, which afforded a clear solution. After stirring under reflux for 5 h, the solution was allowed to cool to room temperature. The solution was washed with 500 ml of water, and the organic phase was removed and concentrated to 50 ml under reduced pressure. After standing for 2 h, the precipitated crystals were filtered off, washed three times with 100 ml of n-hexane and then dried at 70° C. under reduced pressure. The yield at a purity of 99.0% was 47.1 g (90.9%).

後処理

  1. temperatureA suspension, heated
  2. customafforded a clear solution
  3. temperatureunder reflux for 5 h
  4. washThe solution was washed with 500 ml of water
  5. customthe organic phase was removed
  6. concentrationconcentrated to 50 ml under reduced pressure
  7. filtrationthe precipitated crystals were filtered off
  8. washwashed three times with 100 ml of n-hexane
  9. customdried at 70° C. under reduced pressure
  10. customThe yield at a purity of 99.0%

出典と根拠

ORDレコード
ord-2e008cd55780412e8f76fd39668f6b90
出典データセット
uspto-grants-2010_06
特許番号
US07728137B2

関連ノート

読み込み中…