Triphenylphosphine → HCID 21293727、化合物

HRID 622118

反応式

HRID 622118 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 21293727HCID 21293727、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d27479dc65674ab59cc4d7907eef6fa5
出典データセット
uspto-grants-1988_09
特許番号
US04769386

関連ノート

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