Triphenylphosphine → HCID 21293727, 화합물

HRID 622118

반응식

HRID 622118 반응식
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]=[C:13]([CH3:15])[CH3:14].[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>C(#N)C>[Br-:1].[CH3:14][C:13]([CH3:15])=[CH:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][P+:22]([C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 212937251-Bromo-12-methyl-11-tridecene

생성물 1

HCID 21293727HCID 21293727, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1-Bromo-12-methyl-11-tridecene (4.4 g, 16 mmoles) and triphenylphosphine (4.65 g, 17 mmoles) dissolved in acetonitrile (80 ml) were heated to reflux for 4 days, cooled and concentrated in vacuo. The residue was chromatographed on silica gel eluted with chloroform and then with methanol-chloroform (2:3). Fractions containing the product were concentrated in vacuo, triturated with ether, filtered and dried in vacuo to afford the desired phosphonium salt.

후처리

  1. temperaturewere heated
  2. temperatureto reflux for 4 days
  3. temperaturecooled
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed on silica gel
  6. washeluted with chloroform
  7. additionFractions containing the product
  8. concentrationwere concentrated in vacuo
  9. customtriturated with ether
  10. filtrationfiltered
  11. customdried in vacuo

출처 및 근거

ORD 기록
ord-d27479dc65674ab59cc4d7907eef6fa5
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04769386

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