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

HRID 2355

反応式

HRID 2355 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 2631-Butanol触媒HCID 61859Chloroplatinic acid触媒2 回HCID 2631-Butanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f10081548cf4415e81c4b90bffd29a7a
出典データセット
uspto-grants-1998_03
特許番号
US05728857

関連ノート

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