Hydride → 4,4-Ethylenedioxy-3-methyl-1-butanol

HRID 1732279ノート

反応式

HRID 1732279 の反応式
[CH2:1]1[CH2:12][O:11][CH:3]([CH:4]([CH3:10])[CH2:5][C:6](OC)=[O:7])[O:2]1.[Li].[H-].C(=O)(O)[O-].[Na+]>CCOCC>[CH2:1]1[CH2:12][O:11][CH:3]([CH:4]([CH3:10])[CH2:5][CH2:6][OH:7])[O:2]1

参加物

6

反応物 4

HCID 166653HydrideHCID 516892Sodium BicarbonateHCID 3028194LithiumHCID 20305753Methyl 4,4-ethylenedioxy-3-methyl-butanoate

生成物 1

HCID 203057524,4-Ethylenedioxy-3-methyl-1-butanol収率 28.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of methyl 4,4-ethylenedioxy-3-methyl-butanoate (63.2 g) in ether (200 ml) is added dropwise to a mixture of lithium alumnium hydride (13.8 g, 0.363 m) in ether (500 ml) at 0° C. under nitrogen. The resulting mixture is stirred for 2 hours, treated with 5% sodium bicarbonate solution (100 ml), allowed to warm to room temperature and filtered. The filtrate is dried (Na2SO4) and the solvent is evaporated in vacuo to give the crude product (26 g). This material is further purified by column chromatography on silica gel (300 g, 20% ethyl acetate in hexane) to give 4,4-ethylenedioxy-3-methyl-1-butanol as a colorless liquid (14.9 g).

後処理

  1. filtrationfiltered
  2. dry with materialThe filtrate is dried (Na2SO4)
  3. customthe solvent is evaporated in vacuo
  4. customto give the crude product (26 g)
  5. customThis material is further purified by column chromatography on silica gel (300 g, 20% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-c7a6b375c5794b85b18ca5f0bb586559
出典データセット
uspto-grants-1980_12
特許番号
US04237054

反応ノート

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