Water → 2-Propylbutane-1,4-diol

HRID 1788639ノート

反応式

HRID 1788639 の反応式
[CH2:1]([CH:4]([CH2:10][C:11](OCC)=[O:12])[C:5](OCC)=[O:6])[CH2:2][CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[Al]>C(OCC)C>[OH:6][CH2:5][CH:4]([CH2:1][CH2:2][CH3:3])[CH2:10][CH2:11][OH:12]

参加物

6

反応物 4

HCID 962WaterHCID 5359268AluminumHCID 21226445Aluminium lithium hydrideHCID 21856079HCID 21856079、化合物

生成物 1

HCID 125082552-Propylbutane-1,4-diol収率 67%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of diethyl 2-prop-1-ylsuccinate (23.47 g) in diethyl ether (100 ml) was added dropwise to a cooled and stirred suspension of lithium aluminium hydride (6.19 g) in dry diethyl ether (500 ml) under an atmosphere of nitrogen. When the addition was complete, the reaction mixture was stirred at room temperature for 1.5 hours, then enough water to hydrolyse both the excess reducing agent and the intermediate aluminium complexes was added. The resulting solids were filtered off and the filtrate was dried over magnesium sulphate and concentrated to give 3-hydroxymethylhexan-1-ol (9.58 g, 67%) as a colourless oil.

後処理

  1. temperaturea cooled
  2. additionWhen the addition
  3. stirringthe reaction mixture was stirred at room temperature for 1.5 hours
  4. filtrationThe resulting solids were filtered off
  5. dry with materialthe filtrate was dried over magnesium sulphate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c66b4c32006947549b21495daa76d09c
出典データセット
uspto-grants-1987_08
特許番号
US04684396

反応ノート

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