Hydrogen Bromide → (6-Bromo-2-oxohexyl)(triphenyl)phosphanium bromide

HRID 1438830

反応式

HRID 1438830 の反応式
[Br-:1].[O:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=[CH:8][P+:9]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Br>>[Br-:1].[Br:1][CH2:7][CH2:6][CH2:5][CH2:4][C:3](=[O:2])[CH2:8][P+:9]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 73676660[(tetrahydro-2H-pyran-2-ylidene)methyl]triphenylphosphonium bromide

生成物 1

HCID 20369022(6-Bromo-2-oxohexyl)(triphenyl)phosphanium bromide

実験手順

A solution consisting of 1.6 parts of [(tetrahydro-2H-pyran-2-ylidene)methyl]triphenylphosphonium bromide in 25 parts by volume of 48% hydrobromic acid is heated at the reflux temperature for about 5 hours, then is stripped of solvent under reduced pressure to afford the crude product as an amber colored oil. Trituration of that oily material with benzene, followed by evaporation of the benzene under an atmosphere of nitrogen affords (6-bromo-2-oxohexyl)triphenylphosphonium bromide. This product exhibits 60-MHz nuclear magnetic resonance peaks in CDCl3 (deuterated chloroform) at about 100 cps (multiplet), 180 cps (multiplet), 200 cps (multiplet), 357 cps (doublet, J≃12 cps) in addition to the aromatic protons.

後処理

  1. temperatureis heated at the reflux temperature for about 5 hours
  2. customto afford the crude product as an amber colored oil
  3. customTrituration of that oily material with benzene, followed by evaporation of the benzene under an atmosphere of nitrogen

出典と根拠

ORDレコード
ord-107538741cc745ab881bada8e83b57a5
出典データセット
uspto-grants-1977_11
特許番号
US04056562

関連ノート

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