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Methanol → 2,5-Difluoropyridin-4-amine

HRID 1274725
ノート
印刷プレビュー

反応式

HRID 1274725 の反応式
CO.[NH2:3][C:4]1[C:9](Cl)=[C:8]([F:11])[N:7]=[C:6](Cl)[C:5]=1[F:13]>[C].[Pd].C(N(CC)CC)C>[NH2:3][C:4]1[C:5]([F:13])=[CH:6][N:7]=[C:8]([F:11])[CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 887MethanolHCID 221211852,5-Dichloro-3,6-difluoropyridin-4-amine

生成物 1

HCID 221211752,5-Difluoropyridin-4-amine収率 90.8%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 8471Triethylamine溶媒

実験手順

To 40 ml of methanol were added 4.5 g of 4-amino-2,5-dichloro-3,6-difluoropyridine and 4.5 g of triethylamine together with 0.40 g of 10% palladium carbon, and the mixture was hydrogenated at 50° C. for 12 days. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 100 ml of chloroform, and the mixture was washed with 10 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. To the residue were added 1.5 g of triethylamine, 0.35 g of 10% palladium on carbon, and 30 ml of methanol, and the mixture was hydrogenated at 50° C. for 41 hours. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 100 ml of chloroform, and the mixture was washed with 10 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 2.67 g of the title compound as precipitate as a colorless solid.

後処理

  1. customThe catalyst was separated by filtration
  2. distillationthe solvent and the like were distilled off under reduced pressure
  3. additionTo the residue was added 100 ml of chloroform
  4. washthe mixture was washed with 10 ml of distilled water
  5. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionTo the residue were added 1.5 g of triethylamine, 0.35 g of 10% palladium on carbon, and 30 ml of methanol
  8. waitthe mixture was hydrogenated at 50° C. for 41 hours
  9. customThe catalyst was separated by filtration
  10. distillationthe solvent and the like were distilled off under reduced pressure
  11. additionTo the residue was added 100 ml of chloroform
  12. washthe mixture was washed with 10 ml of distilled water
  13. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  14. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-04aafa0d9de14b7abdb44bc11711046e
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06156903

反応ノート

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