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Water → [4-(Benzenesulfonyl)phenyl]phenylphosphinic acid

HRID 2082787
ノート
印刷プレビュー

反応式

HRID 2082787 の反応式
[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13](N)=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F:17][B-:18]([F:21])([F:20])[F:19].[C:22]1([S:28]([C:31]2[CH:36]=[CH:35][C:34]([N+:37]#[N:38])=[CH:33][CH:32]=2)(=[O:30])=[O:29])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.Cl[P:40](Cl)[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1.C(OCC)(=[O:50])C.[OH2:54]>[Cu]Cl>[F:17][B-:18]([F:21])([F:20])[F:19].[C:22]1([S:28]([C:31]2[CH:36]=[CH:35][C:34]([N+:37]#[N:38])=[CH:33][CH:32]=2)(=[O:29])=[O:30])[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1.[C:41]1([P:40]([C:13]2[CH:14]=[CH:15][C:10]([S:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)(=[O:9])=[O:8])=[CH:11][CH:12]=2)(=[O:50])[OH:54])[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 962WaterHCID 8857Ethyl AcetateHCID 12573Phenyl phosphorus dichlorideHCID 5166664-(Phenylsulfonyl)anilineHCID 20360589HCID 20360589、化合物

生成物 2

HCID 20360589HCID 20360589、化合物
HCID 20360606
[4-(Benzenesulfonyl)phenyl]phenylphosphinic acid
収率 45%

試薬・触媒・溶媒 1

HCID 62652Cuprous chloride触媒

実験手順

4-(phenylsulfonyl)benzene diazonium tetrafluoroborate was prepared from 4-aminophenyl phenyl sulfone according to the method of example 11. A slurry of 44 grams of the 4-(phenylsulfonyl)benzenediazonium tetrafluoroborate, 22.8 ml of dichlorophenylphosphine, and 0.5 grams of copper (I) chloride in 400 ml. of ethyl acetate was heated at 30° C for 1.5 hours, cooled, and decomposed by adding 125 ml. of water. The ethyl acetate was removed by steam distillation, and the solid was collected by filtration of the aqueous residue. This solid was extracted with 2 liter of 10% sodium hydroxide, and the extract was acidified with hydrochloric acid to give crude acid. Crystallization from 80% ethanol gave 20 grams (45% yield) of phenyl[4-(phenylsulfonyl)phenyl]phosphinic acid, m.p. 225°-228° C.

後処理

  1. temperaturecooled
  2. additionby adding 125 ml
  3. customThe ethyl acetate was removed by steam distillation
  4. filtrationthe solid was collected by filtration of the aqueous residue
  5. extractionThis solid was extracted with 2 liter of 10% sodium hydroxide
  6. customto give crude acid
  7. customCrystallization from 80% ethanol

出典と根拠

ORDレコード
ord-13e49f5e1df549e1962054d1a7a06e81
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04082793

反応ノート

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