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Acetonitrile → (4-Carboxy-4,4-difluorobutyl)(triphenyl)phosphanium bromide

HRID 569928
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HRID 569928 반응식
C(#N)C.[C:4]1([P:10]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br:23][CH2:24][CH2:25][CH2:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29]>C1(C)C=CC=CC=1>[Br-:23].[C:28]([C:27]([F:32])([F:31])[CH2:26][CH2:25][CH2:24][P+:10]([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1)([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)([OH:30])=[O:29]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 11776TriphenylphosphineHCID 137699515-Bromo-2,2-difluoropentanoic acid

생성물 1

HCID 20146459(4-Carboxy-4,4-difluorobutyl)(triphenyl)phosphanium bromide수율 96.5%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
5 °C

실험 절차

Acetonitrile (23 ml) was added to a mixture of triphenylphosphine (6.7 g, 25.7 mmole) and Part (6) compound (4.6 g, 21.2 mmole). The solution was heated at gentle reflux under magnetic stirring for 30 hours. Toluene (46 ml) was then added and the reaction was brought to reflux for a brief period. The reaction was allowed to cool to 5° C. and kept overnight. The resulting white precipitates were collected, washed with cold acetonitrile/toluene (1/2), and dried in a heated vacuum oven (60° C.~5 mmHg) to give the title bromide (9.8 g, 20.4 mmole, 96.5%) as white solid.

후처리

  1. temperatureThe solution was heated
  2. temperatureat gentle reflux
  3. temperatureto reflux for a brief period
  4. waitkept overnight
  5. customThe resulting white precipitates
  6. customwere collected
  7. washwashed with cold acetonitrile/toluene (1/2)
  8. customdried in a heated vacuum oven (60° C.~5 mmHg)

출처 및 근거

ORD 기록
ord-91203bff665b4ccaac8a33f9f18f443a
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04734424

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