Water → 2-Propylbutane-1,4-diol

HRID 1788639노트

반응식

HRID 1788639 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 5359268AluminumHCID 21226445Aluminium lithium hydrideHCID 21856079HCID 21856079, 화합물

생성물 1

HCID 125082552-Propylbutane-1,4-diol수율 67%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c66b4c32006947549b21495daa76d09c
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04684396

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