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

HRID 1732279노트

반응식

HRID 1732279 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 203057524,4-Ethylenedioxy-3-methyl-1-butanol수율 28.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-c7a6b375c5794b85b18ca5f0bb586559
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04237054

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