Styrene → (2-Phenylethyl)trichlorosilane

HRID 442051

반응식

HRID 442051 반응식
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Cl:9][SiH:10]([Cl:12])[Cl:11].[SiH4]>[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.COC.C=C.C(C1C(C)=CC=C(O)C=1C(C)(C)C)(C)(C)C>[C:3]1([CH2:2][CH2:1][Si:10]([Cl:12])([Cl:11])[Cl:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

8

반응물 3

HCID 7501StyreneHCID 23953SilaneHCID 24811Trichlorosilane

생성물 1

HCID 70327(2-Phenylethyl)trichlorosilane수율 94.2%

시약·촉매·용매 4

HCID 61859Chloroplatinic acid촉매HCID 3034427Phenol, bis(1,1-dimethylethyl)-4-methyl-촉매HCID 6325Ethylene용매HCID 8254Dimethyl Ether용매

반응 조건

온도
90 °C

실험 절차

About 468 grams (4.5 moles) of styrene and about 0.5 grams of di-t-butyl-p-cresol were charged to a one liter, three necked round bottom flask fitted with a magnetic stirrer, thermometer, dropping funnel and reflux condenser bearing a nitrogen by-pass on the vent. While stirring the flask contents were heated to 90° C, and a sufficient amount of about a 2% solution of chloroplatinic acid catalyst dissolved in dimethylether of ethylene glycok to give about 25 parts by weight of plantinum per million parts by weight of reactants was added. Then about 610 grams (4.5 moles) of trichlorosilane were slowly and continuously added via the dropping funnel over a one and one-half hour period while maintaining the reaction temperature at 90°-95° C. A vapor phase chromatogram on the reaction contents indicated there was an essentially complete conversion to product. The crude silane reaction product was then refined by a one plate distillation at 0.1 mm. pressure to yield about 1015 grams (4.24 moles) of phenylethyltrichlorosilane product ##STR22## (94.5% conversion) which had a boiling point of about 63°-64° C./0.1 mm Hg.

후처리

  1. customfitted with a magnetic stirrer
  2. temperaturereflux condenser
  3. customto give about 25 parts by weight of plantinum per million parts by weight of reactants
  4. additionwas added
  5. additioncontinuously added via the dropping funnel over a one and one-half hour period
  6. temperaturewhile maintaining the reaction temperature at 90°-95° C
  7. customA vapor phase chromatogram on the reaction contents
  8. distillationwas then refined by a one plate distillation at 0.1 mm

출처 및 근거

ORD 기록
ord-00e0f416c9bb42c99dc3dae430b350ce
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04044037

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