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

HRID 1656302

反応式

HRID 1656302 の反応式
[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

参加物

4

反応物 2

HCID 962WaterHCID 9006Dichloromethylphenylsilane2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-14308a76c04a49a8adc4d2815ebec256
出典データセット
uspto-grants-1993_10
特許番号
US05254439

関連ノート

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