2-Methyl-3-buten-2-ol → 1,1-Dimethyl-3-(triethylsilyl)propyl alcohol

HRID 2355

반응식

HRID 2355 반응식
[CH3:1][C:2]([OH:6])([CH3:5])[CH:3]=[CH2:4].[CH2:7]([SiH:9]([CH2:12][CH3:13])[CH2:10][CH3:11])[CH3:8]>[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.C(O)CCC>[CH3:1][C:2]([OH:6])([CH3:5])[CH2:3][CH2:4][Si:9]([CH2:12][CH3:13])([CH2:10][CH3:11])[CH2:7][CH3:8]

참가 물질

6

반응물 2

HCID 82572-Methyl-3-buten-2-olHCID 12052Triethylsilane

생성물 1

HCID 537862691,1-Dimethyl-3-(triethylsilyl)propyl alcohol수율 81.1%

시약·촉매·용매 3

HCID 2631-Butanol촉매HCID 61859Chloroplatinic acid촉매2회HCID 2631-Butanol용매

반응 조건

온도
80 °C

실험 절차

Into a four-necked 500 mL-flask equipped with a stirring apparatus, a thermometer and a dropping funnel, 81.2 g (0.943 mole) of 3-methyl-1-buten-3-ol and 0.2 g of an n-butanol solution containing chloroplatinic acid at a concentration of 2 weight % were charged, and they were heated to 80° C. with stirring. From the dropping funnel, 109.6 g (0.943 mole) of triethylsilane was dropwise added into the four-necked flask. After the completion of the addition, they were heated and stirred for about 20 hours. Meanwhile, the proceeding of reaction was traced by gas chromatography analysis. At the stage when the proceeding of the reaction stopped, an additional mount of the above n-butanol solution containing chloroplatinic acid was added for the proceeding of the reaction. The reaction mixture was distilled under reduced pressure to obtain 154.9 g (0.765 mole) of 1,1-dimethyl-3-(triethylsilyl)propyl alcohol as a fraction at 105° C./14-16 torr.

후처리

  1. customInto a four-necked 500 mL-flask equipped with a stirring apparatus
  2. additionwere charged
  3. additionAfter the completion of the addition, they
  4. temperaturewere heated
  5. stirringstirred for about 20 hours
  6. customMeanwhile, the proceeding of reaction
  7. additionwas added for the proceeding of the reaction
  8. distillationThe reaction mixture was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-f10081548cf4415e81c4b90bffd29a7a
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728857

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