Triphenylphosphine → {4[(1E)-3-ethoxy-3-oxoprop-1-enyl]-3-methylbenzyl}(triphenyl)phosphonium bromide

HRID 9633

反応式

HRID 9633 の反応式
[Br:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[C:5]([CH3:16])[CH:4]=1.[C:17]1([P:23]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C1(C)C=CC=CC=1>[Br-:1].[CH2:14]([O:13][C:11](=[O:12])/[CH:10]=[CH:9]/[C:6]1[CH:7]=[CH:8][C:3]([CH2:2][P+:23]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[CH:4][C:5]=1[CH3:16])[CH3:15]

参加物

4

反応物 2

HCID 11776Triphenylphosphine2 回HCID 21986333Ethyl(2E)-3-[4-(bromomethyl)-2-methylphenyl]prop-2-enoate2 回

生成物 1

HCID 87902646{4[(1E)-3-ethoxy-3-oxoprop-1-enyl]-3-methylbenzyl}(triphenyl)phosphonium bromide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of ethyl(2E)-3-[4-(bromomethyl)-2-methylphenyl]prop-2-enoate (intermediate 20, 1.494 g) in toluene (30 ml) was stirred and treated with triphenylphosphine (1.52 g) and then heated at reflux for 2 hours then at 21° C. overnight. More triphenylphosphine (0.5 g) was then added and the reaction heated at reflux for a further 5 hours. The mixture was then allowed to cool and filtered to give the title compound as a white solid.

後処理

  1. temperatureheated
  2. temperatureat reflux for 2 hours
  3. customat 21° C.
  4. customovernight
  5. temperaturethe reaction heated
  6. temperatureat reflux for a further 5 hours
  7. temperatureto cool
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-32763027959a429c81902ee9b65452a4
出典データセット
uspto-grants-2006_08
特許番号
US07091237B2

関連ノート

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