Potassium Carbonate → HCID 21553923、化合物

HRID 267793

反応式

HRID 267793 の反応式
[Cl:1][C:2]1[CH:9]=[C:6]([CH:7]=[O:8])[C:5]([OH:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH:18]([CH3:21])[C:19]#[N:20]>CC(C)=O>[Cl:1][C:2]1[CH:9]=[C:6]([C:5]([O:10][CH:18]([C:19]#[N:20])[CH3:21])=[CH:4][CH:3]=1)[CH:7]=[O:8]

参加物

5

反応物 3

HCID 11430Potassium Carbonate2 回HCID 124815-Chloro-salicylaldehydeHCID 5192252-Chloropropionitrile2 回

生成物 1

HCID 21553923HCID 21553923、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 5-chlorosalicylaldehyde (78 g., 0.5 mole), finely powdered anhydrous potassium carbonate (103.5 g., 0.75 mole) and acetone (500 ml.) is stirred under reflux and 2-chloropropionitrile (33.6 g., 0.375 mole) is added over a period of about 5 minutes. The mixture is heated under reflux for 1.5 hours and then treated with potassium carbonate (34.5 g., 0.25 mole) followed by more 2-chloropropionitrile (11.2 g., 0.125 mole). Heating and stirring are continued for 31/2 hours, after which the reaction mixture is filtered and the filter-cake washed with acetone. Evaporation of the combined filtrate gives 3-chloro-6-(1-cyanoethoxy)-benzaldehyde which is recrystallized from aqueous methanol.

後処理

  1. temperatureunder reflux
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 1.5 hours
  4. temperatureHeating
  5. stirringstirring
  6. custom2 hours
  7. filtrationafter which the reaction mixture is filtered
  8. washthe filter-cake washed with acetone
  9. customEvaporation of the combined filtrate

出典と根拠

ORDレコード
ord-7a6b98e1ac1041ad9fec417b3c3d37b2
出典データセット
uspto-grants-1976_03
特許番号
US03944560

関連ノート

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