Acetic Acid → 3-Chloro-4,4-diethoxybutan-2-one

HRID 1979804노트

반응식

HRID 1979804 반응식
[Na].Cl[CH:3]=[C:4]([Cl:8])[C:5](=[O:7])[CH3:6].[C:9]([OH:12])(=O)[CH3:10].[CH2:13]([OH:15])[CH3:14]>>[Cl:8][CH:4]([C:5](=[O:7])[CH3:6])[CH:3]([O:12][CH2:9][CH3:10])[O:15][CH2:13][CH3:14]

참가 물질

5

반응물 4

HCID 176Acetic AcidHCID 702Ethanol2회HCID 5360545SodiumHCID 534251373,4-Dichlorobut-3-en-2-one

생성물 1

HCID 127217263-Chloro-4,4-diethoxybutan-2-one수율 64%

실험 절차

To a solution of 2.30 g of sodium metal in 180 ml ethanol, cooled in an ice-bath is added dropwise a solution of 13.90 g (0.10 mole) 1,2-dichloro-1-buten-3-one in 20 ml ethanol. The mixture is stirred for 2 hours, acidified with glacial acetic acid (4 ml) and the precipitated salt removed by filtration, washing with ethanol. The filtrate is concentrated in vacuo, the residue slurried in ethyl ether and filtered to remove salt. The ether is evaporated in vacuo and the residual oil is distilled to yield 12.49 g (64%) of the title compound, B.P. 52° C. at 1.5 torr. 1H-NMR (CDCl3) ppm (delta): 1.17 (t, 3H), 1.22 (t, 3H), 2.30 (s, 3H), 3.63 (m, 4H), 4.18 (d, 1H), 4.68 (d, 1H).

후처리

  1. customthe precipitated salt removed by filtration
  2. washwashing with ethanol
  3. concentrationThe filtrate is concentrated in vacuo
  4. filtrationfiltered
  5. customto remove salt
  6. customThe ether is evaporated in vacuo
  7. distillationthe residual oil is distilled

출처 및 근거

ORD 기록
ord-93cdd7206e5b410b8e343887b7d91f34
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482723

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