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Water → HCID 178454801, 화합물

HRID 1292574
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HRID 1292574 반응식
[CH:1]1[CH:6]=[CH:5][C:4]([P-:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.[K+].F[C:16]1[CH:21]=[CH:20][C:19]([CH2:22][PH:23](=[O:29])[O:24][CH2:25][CH:26]([CH3:28])[CH3:27])=[CH:18][CH:17]=1.O>C1COCC1>[C:8]1([P:7]([C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)[C:16]2[CH:21]=[CH:20][C:19]([CH2:22][PH:23](=[O:29])[O:24][CH2:25][CH:26]([CH3:28])[CH3:27])=[CH:18][CH:17]=2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 11042360KPPh2HCID 178454800HCID 178454800, 화합물

생성물 1

HCID 178454801HCID 178454801, 화합물수율 98.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
23 °C

실험 절차

200 ml (100 mmol) of potassium diphenylphosphide solution in THF (manufacturer: Aldrich) were added dropwise at -5° C. to a solution of 21.90 g (95 mmol) of isobutyl 4-fluorophenylmethylphosphinate in 150 ml of THF. After stirring for 20 hours at 23° C., the mixture was hydrolyzed by addition of 250 ml of degassed water and stirring for 15 minutes. Extraction with ethyl acetate, drying of the organic phase over Na2SO4, evaporation on a rotary evaporator and drying under reduced pressure gave 37.0 g of isobutyl (4-diphenylphosphinophenyl)methylphosphinate in the form of a yellow oil.

후처리

  1. stirringstirring for 15 minutes
  2. extractionExtraction with ethyl acetate
  3. dry with materialdrying of the organic phase over Na2SO4, evaporation on a rotary evaporator
  4. customdrying under reduced pressure

출처 및 근거

ORD 기록
ord-9d471c0e270d40a5b0d8ed716dbc9061
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05756804

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