Pentamethyldisiloxane → 4-Cyanophenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate

HRID 1197723

反応式

HRID 1197723 の反応式
[CH2:1]([O:7][C:8]1[CH:24]=[CH:23][C:11]([C:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[CH:17][CH:16]=2)=[O:13])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH2:4][CH:5]=[CH2:6].[CH3:25][SiH:26]([CH3:32])[O:27][Si:28]([CH3:31])([CH3:30])[CH3:29]>C1(C)C=CC=CC=1.C1([Pt](Cl)(Cl)C2C=CC=C2)C=CC=C1>[CH3:25][Si:26]([CH3:32])([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH2:1][O:7][C:8]1[CH:24]=[CH:23][C:11]([C:12]([O:14][C:15]2[CH:16]=[CH:17][C:18]([C:21]#[N:22])=[CH:19][CH:20]=2)=[O:13])=[CH:10][CH:9]=1)[O:27][Si:28]([CH3:31])([CH3:30])[CH3:29]

参加物

5

反応物 2

HCID 74037PentamethyldisiloxaneHCID 1822389Benzoic acid, 4-(5-hexenyloxy)-, 4-cyanophenyl ester

生成物 1

HCID 199721604-Cyanophenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate

試薬・触媒・溶媒 2

HCID 178479810HCID 178479810、化合物触媒2 回HCID 1140Toluene溶媒

実験手順

0.94 g (0.024 mmol of Pt) of 0.5% strength dicyclopentadienylplatinum dichloride solution (dichloromethane) was added to a solution of 13.8 g (42.9 mmol) of 4-cyanophenyl 4-(5-hexenyloxy)benzoate and 6.48 g (43.7 mmol) of pentamethyldisiloxane in 50.0 g of toluene, and the mixture was refluxed for 3 hours. After complete hydrosilylation of the olefin, a further 0.94 g (0.024 mmol of Pt) of 0.5% strength dicyclopentadienylplatinum dichloride solution (dichloromethane) were added, and the mixture was refluxed for a further 2 hours. The reaction mixture was flushed with nitrogen, and the toluene was removed by vacuum distillation on a rotary evaporator. The crude product was purified by chromatography on silica gel. The 4-cyanophenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate obtained was additionally recrystallized from petroleum ether (100° C.-140° C.) and exhibited the following phase behavior: c 54-55 (sA 53-55) i.

後処理

  1. temperaturethe mixture was refluxed for 3 hours
  2. temperaturethe mixture was refluxed for a further 2 hours
  3. customThe reaction mixture was flushed with nitrogen
  4. customthe toluene was removed by vacuum distillation on a rotary evaporator
  5. customThe crude product was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-5723a77c7f4f4bf3a0a6d26b44f3fc07
出典データセット
uspto-grants-1994_01
特許番号
US05277838

関連ノート

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