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

HRID 27354노트

반응식

HRID 27354 반응식
[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

참가 물질

5

반응물 3

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

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-methylbutanoate (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).

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-eb178ed36c2c47eea34d97508000c9b4
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221717

반응 노트

불러오는 중…