Water → Disiloxane, 1,3-dichloro-1,3-dimethyl-1,3-diphenyl-

HRID 893778

반응식

HRID 893778 반응식
[CH3:1][Si:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(Cl)[Cl:3].[OH2:11]>CCOCC>[CH3:1][Si:2]([Cl:3])([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[O:11][Si:2]([Cl:3])([CH3:1])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 9006Dichloromethylphenylsilane2회

생성물 1

HCID 107420Disiloxane, 1,3-dichloro-1,3-dimethyl-1,3-diphenyl-수율 33.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

Methylphenyl dichlorosilane (765 g; 4.0 mol.) and the same amount of diethyl ether were introduced into a four-necked flask of 2 liters volume equipped with a stirring machine, a reflux condenser, a thermometer and a dropping funnel, followed by stirring the mixture, dropwise adding 36 g (2.0 mol.) of water through the dropping funnel over five hours under nitrogen atmosphere, and then refluxing the mixture for an additional three hours. After refluxing the mixture, ether was distilled off and the starting material, methylphenyl dichlorosilane (184 g; 0.96 mol.) was recovered by distilling the reaction mixture in vacuo to obtain 220 g (0.67 mol.) of 1,3-dimethyl-1,3-diphenyl dichlorodisiloxane. Boiling Point=135°-138° C./2 mmHg.

후처리

  1. customequipped with a stirring machine, a reflux condenser
  2. temperaturerefluxing the mixture for an additional three hours
  3. distillationwas distilled off
  4. distillationby distilling the reaction mixture in vacuo

출처 및 근거

ORD 기록
ord-f8a413fbb0db4da2bc93d96bc94bf984
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05126419

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