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Methanol → 2-(t-Butylamino)-5-chloro-3,6-difluoropyridine

HRID 610221
ノート
印刷プレビュー

反応式

HRID 610221 の反応式
CO.Br[C:4]1[C:9]([Cl:10])=[C:8]([F:11])[N:7]=[C:6]([NH:12][C:13]([CH3:16])([CH3:15])[CH3:14])[C:5]=1[F:17]>[Pd].C(N(CC)CC)C>[C:13]([NH:12][C:6]1[C:5]([F:17])=[CH:4][C:9]([Cl:10])=[C:8]([F:11])[N:7]=1)([CH3:16])([CH3:14])[CH3:15]
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 221211704-Bromo-2-(t-butylamino)-5-chloro-3,6-difluoropyridine

生成物 1

HCID 221211892-(t-Butylamino)-5-chloro-3,6-difluoropyridine収率 98.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8471Triethylamine溶媒

実験手順

To 30 ml of methanol were added 12.8 g of 4-bromo-2-(t-butylamino)-5-chloro-3,6-difluoropyridine and 2.5 g of triethylamine together with 0.57 g of 10% palladium on carbon, and the mixture was hydrogenated at 50° C. for 5 days. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 80 ml of chloroform, and the mixture was washed with 70 ml of distilled water, and the chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 9.3 g of the title compound as a brown oil.

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 80 ml of chloroform
  4. washthe mixture was washed with 70 ml of distilled water
  5. dry with materialthe chloroform layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-667ff37515af48358fc5cd7d0b018db3
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998436

反応ノート

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