Dimethylphenylsilane → Dimethyl-3-(2'-methyl-3'-cyanophenyl)-propylphenylsilane

HRID 1656930

반응식

HRID 1656930 반응식
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH:10]=[CH2:11])[C:4]=1[CH3:12])#[N:2].[CH3:13][SiH:14]([CH3:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>C1CCCCC1.C(O)(C)C.O.Cl.Cl.Cl[Pt](Cl)(Cl)Cl>[CH3:13][Si:14]([CH3:21])([CH2:11][CH2:10][CH2:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:1]#[N:2])[C:4]=1[CH3:12])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 2

HCID 13014DimethylphenylsilaneHCID 197864851-Cyano-2-methyl-3-prop-2-enylbenzene

생성물 1

HCID 19786496Dimethyl-3-(2'-methyl-3'-cyanophenyl)-propylphenylsilane수율 73.1%

시약·촉매·용매 3

HCID 16211507Platinate(2-), hexachloro-, hydrogen, hydrate (1:2:1), (OC-6-11)-촉매HCID 3776Isopropanol용매HCID 8078Cyclohexane용매

반응 조건

온도
55 °C

실험 절차

9.0 g of 1-cyano-2-methyl-3-prop-2-enylbenzene are dissolved in 100 ml of absolute cyclohexane, and 7.75 g of dimethylphenylsilane are added at room temperature. 0.1 g of hexachloroplatinic acid hexahydrate, dissolved in 2 ml of absolute isopropanol, is added to this mixture. The reaction mixture is stirred for 3 hours at 55° C. The solvent is removed by distillation in a rotary evaporator. High boiling components are separated off by distillation under reduced pressure (condensate 82°-105° C./0.1 mbar). The residue is purified by column chromatography (silica gel/toluene). 12.2 g of dimethyl-3-(2'-methyl-3'-cyanophenyl)-propylphenylsilane are obtained.

후처리

  1. additionis added to this mixture
  2. customThe solvent is removed by distillation in a rotary evaporator
  3. customare separated off by distillation under reduced pressure (condensate 82°-105° C./0.1 mbar)
  4. customThe residue is purified by column chromatography (silica gel/toluene)

출처 및 근거

ORD 기록
ord-8e79860bd1564b1ebdde728909d9ad0d
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256666

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