Potassium Carbonate → 2-chloro-N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2-difluoroacetamide

HRID 1851688ノート

反応式

HRID 1851688 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][N:3]=1.[Cl:10][C:11]([F:22])([F:21])[C:12]([N:14]=[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][NH:16]1)=[O:13].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:10][C:11]([F:21])([F:22])[C:12]([N:14]=[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N:16]1[CH2:8][C:5]1[CH:4]=[N:3][C:2]([Cl:1])=[CH:7][CH:6]=1)=[O:13]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 1554792-Chloro-5-(chloromethyl)pyridineHCID 178522124HCID 178522124、化合物

生成物 1

HCID 866869322-chloro-N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2-difluoroacetamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

An amount of 53 mg (0.33 mmol) of 2-chloro-5-chloromethylpyridine dissolved in 6 mL of anhydrous acetonitrile was added to 68 mg (0.33 mmol) of 2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide synthesized by the above method, following which 50 mg (0.36 mmol) of potassium carbonate was added and refluxing under heating was carried out for 1 hour. Following reaction completion, the reaction mixture was returned to room temperature then concentrated under reduced pressure. Diethyl ether was added to the concentrate, whereupon a solid separated out. The solid was collected by filtration and dried, affording the target compound in an amount of 49 mg (yield, 45%).

後処理

  1. customsynthesized by the above method
  2. additionwas added
  3. temperaturerefluxing
  4. temperatureunder heating
  5. customreaction completion
  6. customwas returned to room temperature
  7. concentrationthen concentrated under reduced pressure
  8. additionDiethyl ether was added to the concentrate, whereupon a solid
  9. customseparated out
  10. filtrationThe solid was collected by filtration
  11. customdried
  12. customaffording the target compound
  13. customin an amount of 49 mg (yield, 45%)

出典と根拠

ORDレコード
ord-c0a5df7b53b74b839f315953f9da90f5
出典データセット
uspto-grants-2015_02
特許番号
US08957214B2

反応ノート

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