Sodium Hydroxide → 4-Diphenylphosphinophenylphosphonic Acid

HRID 2392847ノート

反応式

HRID 2392847 の反応式
[OH-].[Na+].[C:3]1([P:9]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:10]2[CH:15]=[CH:14][C:13]([P:16](=[O:23])([O:20]CC)[O:17]CC)=[CH:12][CH:11]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>O.C1COCC1.Cl>[C:24]1([P:9]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:10]2[CH:15]=[CH:14][C:13]([P:16](=[O:17])([OH:20])[OH:23])=[CH:12][CH:11]=2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

参加物

6

反応物 2

HCID 14798Sodium HydroxideHCID 15243843Diethyl [4-(diphenylphosphanyl)phenyl]phosphonate

生成物 1

HCID 112678574-Diphenylphosphinophenylphosphonic Acid

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
23 °C

実験手順

0.40 g (10.0 mmol) of NaOH in 7 ml of water are added dropwise at 23° C. to a solution of 2.00 g (5.0 mmol) of diethyl 4-diphenylphosphinophenylphosphonate in 7 ml of THF. After refluxing for 6 hours, the mixture is diluted with a further 7 ml of THF, 4.0 ml of 2N hydrochloric acid are added dropwise at 23° C. and the mixture is stirred for 20 min at 23° C. After phase separation, the aqueous phase is extracted twice, each time with 25 ml of dichloromethane, and the combined organic phases are washed with 25 ml of water. After drying over Na2SO4, complete evaporation on a rotary evaporator and drying under reduced pressure, 1.54 g of 4-diphenylphosphinophenylphosphonic acid (90% of theory) are obtained in the form of a pale yellow solid having an m.p. of 87° C.

後処理

  1. temperatureAfter refluxing for 6 hours
  2. additionare added dropwise at 23° C.
  3. customAfter phase separation
  4. extractionthe aqueous phase is extracted twice
  5. washeach time with 25 ml of dichloromethane, and the combined organic phases are washed with 25 ml of water
  6. dry with materialAfter drying over Na2SO4, complete evaporation on a rotary evaporator
  7. dry with materialdrying under reduced pressure, 1.54 g of 4-diphenylphosphinophenylphosphonic acid (90% of theory)
  8. customare obtained in the form of a pale yellow solid

出典と根拠

ORDレコード
ord-fafa1177271940568f49f6fd336a118d
出典データセット
uspto-grants-1998_09
特許番号
US05801263

反応ノート

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