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

HRID 1979804ノート

反応式

HRID 1979804 の反応式
[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]

参加物

5

反応物 4

HCID 176Acetic AcidHCID 702Ethanol2 回HCID 5360545SodiumHCID 534251373,4-Dichlorobut-3-en-2-one

生成物 1

HCID 127217263-Chloro-4,4-diethoxybutan-2-one収率 64%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-93cdd7206e5b410b8e343887b7d91f34
出典データセット
uspto-grants-1984_11
特許番号
US04482723

反応ノート

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