Sodium Bicarbonate → 4,4-Ethylenedioxy-3-methyl-1-butanol

HRID 2051727ノート

反応式

HRID 2051727 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.[H-].[Al+3].[Li+].[H-].[H-].[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

5

反応物 3

HCID 516892Sodium BicarbonateHCID 20305753Methyl 4,4-ethylenedioxy-3-methyl-butanoateHCID 21226445Aluminium lithium hydride

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 aluminum hydride (13.8 g, 0.363 m) in ether (500 ml) at 0° C. under nitrogen. The resulting mixture is stirred for 2 hr., 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-bcd2dadf7ab04c92ae4ee4b1c2e2e516
出典データセット
uspto-grants-1980_01
特許番号
US04182717

反応ノート

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