p-Toluenesulfonic acid monohydrate → HCID 178418333、化合物

HRID 1403

反応式

HRID 1403 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][CH:10](O)[CH2:11][C@H:12]2[CH2:17][CH2:16][Si@H:15]([CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]#[C:9]/[CH:10]=[CH:11]/[C@H:12]2[CH2:13][CH2:14][Si@H:15]([CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:16][CH2:17]2)=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 178418481HCID 178418481、化合物

生成物 1

HCID 178418333HCID 178418333、化合物収率 15.9%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 1-(4-fluorophenyl)-4-(trans-4-pentyl-4-silacyclohexyl)-1-butyne-3-ol 8.0 g (24 mmol), p-toluenesulfonic acid monohydrate 1.6 g, and benzene 200 ml was heated under reflux to remove the water and then subjected to a conventional post-treatment. The reaction mixture thus obtained was not only a mixture of trans- and cis-isomers, with respect to the silacyclohexane ring, but also a mixture of E- and Z-isomers, with respect to the double bond. Hence, the product was separated by chromatography to give 1.2 g of the desired product of the trans-E isomer (yield 15.9%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. customto remove the water
  4. customThe reaction mixture thus obtained
  5. additiona mixture of trans- and cis-isomers
  6. additionwith respect to the silacyclohexane ring, but also a mixture of E- and Z-isomers
  7. customHence, the product was separated by chromatography

出典と根拠

ORDレコード
ord-62dac6c13c4c4aa59ca7877a94095e3c
出典データセット
uspto-grants-1998_03
特許番号
US05725797

関連ノート

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