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Triphenylphosphine → 3-(4-Ethoxy-2,3-difluorophenyl)propyltriphenylphosphonium bromide

HRID 2039369
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HRID 2039369 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][Br:13])=[C:6]([F:14])[C:5]=1[F:15])[CH3:2].[C:16]1([P:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C1(C)C=CC=CC=1>[Br-:13].[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][P+:22]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)=[C:6]([F:14])[C:5]=1[F:15])[CH3:2]
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참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 22913643HCID 22913643, 화합물

생성물 1

HCID 866684593-(4-Ethoxy-2,3-difluorophenyl)propyltriphenylphosphonium bromide수율 78.9%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
25 °C

실험 절차

3-(4-Ethoxy-2,3-difluorophenyl)bromopropane (s22) (11.5 g), toluene (100 ml) and triphenylphosphine (21.6 g) were placed in a reaction vessel under an atmosphere of nitrogen, and the mixture was heated to reflux for 5 hours. After the reaction mixture had been cooled to 25° C., the deposits were filtered, and the unreacted material was removed by washing with toluene three times. The resulting colorless solids were dried to give 3-(4-ethoxy-2,3-difluorophenyl)propyltriphenylphosphonium bromide (s23) (17.6 g). The yield based on the compound (s22) was 78.9%.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 5 hours
  3. filtrationthe deposits were filtered
  4. customthe unreacted material was removed
  5. washby washing with toluene three times
  6. customThe resulting colorless solids were dried

출처 및 근거

ORD 기록
ord-614171ea941d4da4ba03a9bd037ad63c
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08580146B2

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