Ethanol → N-(2,4-Dimethylphenyl)-3-oxobutanamide

HRID 259964

反応式

HRID 259964 の反応式
[CH3:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH2:4].[CH2:10]=[C:11]1[O:15][C:13](=[O:14])[CH2:12]1.C(O)C>O>[CH3:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH:4][C:13](=[O:14])[CH2:12][C:11]([CH3:10])=[O:15]

参加物

5

反応物 3

HCID 702EthanolHCID 72502,4-DimethylanilineHCID 12661Diketene

生成物 1

HCID 222464N-(2,4-Dimethylphenyl)-3-oxobutanamide収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
85 °C

実験手順

2.48 kg/h (20.5 mol/h) of 2,4-dimethylaniline, 1.83 kg/h (21.3 mol/h) of diketene (purity 98%) and 8 kg/h of a mixture of 2.4 kg/h of ethanol and 5.6 kg/h of water are metered separately but simultaneously into a reactor which has been preheated to about 80° C. The reactor consists of a double-shell glass vessel of about 0.6 l capacity and is equipped with a stirrer, thermometer, reflux condenser and, at the bottom, with a run-off. Immediately the metering has started, the heat evolved by the reaction causes the reactor contents to reflux at about 85° C. The heating of the reactor is discontinued and the reaction is continued by limiting the reactor contents to about 0.3 1 by continuous pumping out. The reactor discharge is cooled to about 15° C. with stirring, and the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration. The moist product, which is obtained at about 5 kg/h, is washed with about 4 kg/h of cold aqueous 30% strength ethanol and dried, leaving 4 kg/h (19.5 mol/h) of 2',4'-dimethylacetoacetanilide (melting point about 89° C.) corresponding to a yield of 95% based on amine.

後処理

  1. customare metered separately but simultaneously into a reactor
  2. customhas been preheated to about 80° C
  3. customThe reactor consists of a double-shell glass vessel of about 0.6 l capacity
  4. customis equipped with a stirrer
  5. temperaturethermometer, reflux condenser
  6. temperatureThe heating of the reactor
  7. temperatureThe reactor discharge is cooled to about 15° C.
  8. customthe light-colored crystals which are formed
  9. customare separated from about 7 kg/h of the pale yellow mother liquor by filtration
  10. customThe moist product, which is obtained at about 5 kg/h
  11. washis washed with about 4 kg/h of cold aqueous 30% strength ethanol
  12. customdried

出典と根拠

ORDレコード
ord-dcb83adae09b473c97bc728e6804a512
出典データセット
uspto-grants-1996_06
特許番号
US05523486

関連ノート

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