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

HRID 1197722

Reaktionsgleichung

Reaktionsgleichung von HRID 1197722
[CH2:1]([O:7][C:8]1[CH:31]=[CH:30][C:11]([C:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:17][CH:16]=2)=[O:13])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH2:4][CH:5]=[CH2:6].[CH3:32][SiH:33]([CH3:39])[O:34][Si:35]([CH3:38])([CH3:37])[CH3:36]>C1(C)C=CC=CC=1.C1([Pt](Cl)(Cl)C2C=CC=C2)C=CC=C1>[CH3:32][Si:33]([CH3:39])([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH2:1][O:7][C:8]1[CH:31]=[CH:30][C:11]([C:12]([O:14][C:15]2[CH:16]=[CH:17][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:19][CH:20]=2)=[O:13])=[CH:10][CH:9]=1)[O:34][Si:35]([CH3:38])([CH3:37])[CH3:36]

Komponenten

5

Edukt 2

HCID 74037PentamethyldisiloxaneHCID 148478754-Octyloxyphenyl 4-(5-hexenyloxy)benzoate

Produkt 1

HCID 191045044-Octyloxyphenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178479810HCID 178479810, VerbindungKatalysatorHCID 1140TolueneLösungsmittel

Versuchsvorschrift

0.94 g (0.024 mmol of Pt) of 0.5% strength dicyclopentadienylplatinum dichloride solution (dichloromethane) was added to a solution of 20.0 g (47.2 mmol) of 4-octyloxyphenyl 4-(5-hexenyloxy)benzoate and 7.10 g (48.0 mmol) of pentamethyldisiloxane in 20.0 g of toluene, and the mixture was refluxed for 5 hours. After complete hydrosilylation of the olefin, 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-octyloxyphenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate obtained was additionally recrystallized from ethanol and exhibited the following phase behavior: c 38 s 50 i.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-6f622f0800c146ecbde1edf511cd27e2
Quelldatensatz
uspto-grants-1994_01
Patentnummer
US05277838

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