1,2-Diethenylbenzene → (2-Dichloromethylsilyl-ethyl)styrene

HRID 1387608

반응식

HRID 1387608 반응식
C(C1C=CC=CC=1C=C)=C.[CH2:11]([CH:13]=[CH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH3:12].[Cl:21][CH:22]([SiH3:24])[Cl:23]>>[Cl:21][CH:22]([SiH2:24][CH2:12][CH2:11][CH:13]=[CH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[Cl:23]

참가 물질

4

반응물 3

HCID 666661,2-DiethenylbenzeneHCID 1230881-Phenyl-1-buteneHCID 57353436(Dichloromethyl)silane2회

생성물 1

HCID 131722819(2-Dichloromethylsilyl-ethyl)styrene

실험 절차

A 500 ml three-neck, round bottom flask equipped with a magnetic stirrer, a condenser and an addition funnel was charged with 60 ml (0.337 mol) of divinylbenzene (Aldrich Chemical Co., Milwaukee, Wis.); mixture of 80% m- and p- isomers and 20% ethylvinylbenzene) under an argon atmosphere and at room temperature (RT). While stirring, 200 ml of distilled and dried hexanes were added followed by 0.5 ml of the above described platinum catalyst solution (SIP6830.0 from Gelest). Dichloromethylsilane (39.0 ml; 0.371 mol) was placed in the addition funnel, the argon supply was disrupted and a drying tube was attached to the system. The dichloromethylsilane was added dropwise at room temperature and the reaction was monitored by 1H NMR spectroscopy. After 48 hours, it was determined that hydrosilation was complete, the addition funnel and condenser were replaced by a distillation head and the crude product was purified by fractional distillation. The desired product was obtained as a mixture, 77% thereof corresponding to a combination of meta- and para-(2-dichloromethylsilyl-ethyl)-styrene (DSiSt) of the formula

후처리

  1. customA 500 ml three-neck, round bottom flask equipped with a magnetic stirrer, a condenser and an addition funnel
  2. additionmixture of 80% m-
  3. customat room temperature
  4. custom(RT)
  5. distillation200 ml of distilled
  6. additiondried hexanes were added
  7. customa drying tube was attached to the system
  8. distillationthe crude product was purified by fractional distillation

출처 및 근거

ORD 기록
ord-f08305c2c4a74ce7a69aae05166dc75b
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06268451B1

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