Sodium Hydroxide → Tetra-n-butylphosphonium Diphenylphosphinate

HRID 614578

반응식

HRID 614578 반응식
[C:1]1([P:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)(=[O:9])[OH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>O.[Cl-].C([P+](CCCC)(CCCC)CCCC)CCC>[C:1]1([P:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)(=[O:8])[O-:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1.[CH2:6]([P+:7]([CH2:1][CH2:6][CH2:5][CH3:4])([CH2:10][CH2:15][CH2:14][CH3:13])[CH2:15][CH2:10][CH2:11][CH3:12])[CH2:1][CH2:2][CH3:3]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 15567Diphenylphosphinic acid

생성물 1

HCID 21328170Tetra-n-butylphosphonium Diphenylphosphinate

시약·촉매·용매 2

HCID 75311Tetrabutylphosphonium chloride촉매HCID 962Water용매3회

실험 절차

To a suspension of 43.6 grams of diphenylphosphinic acid in 300 milliliters of distilled water is added a solution of 8.0 grams of sodium hydroxide in 200 milliliters of water and the mixture stirred. The acid dissolves slowly. To the resulting solution is added a solution of 59 grams of tetra-n-butylphosphonium chloride in about 200 milliliters of distilled water. The reaction mixture is stirred for half an hour and is then extracted with about 500-milliliter portion of chloroform. The extract is dried over anhydrous Na2SO4 and the chloroform is then distilled. A light-brown viscous liquid remains. It is dried overnight at 80° C. On cooling, tetra-n-butylphosphonium diphenylphosphinate separates as white crystals.

후처리

  1. dissolutionThe acid dissolves slowly
  2. stirringThe reaction mixture is stirred for half an hour
  3. extractionis then extracted with about 500-milliliter portion of chloroform
  4. dry with materialThe extract is dried over anhydrous Na2SO4
  5. distillationthe chloroform is then distilled
  6. customIt is dried overnight at 80° C
  7. temperatureOn cooling

출처 및 근거

ORD 기록
ord-273dc3e8c39646b89cee53365222f12e
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04145473

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