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Methanol → 2-Amino-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine

HRID 368512
ノート
印刷プレビュー

反応式

HRID 368512 の反応式
CO.[NH2:3][C:4]1[C:9]([F:10])=[C:8]([Br:11])[C:7](Cl)=[C:6]([NH:13][C:14]([CH3:21])([CH3:20])[CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])[N:5]=1>[Pd].C(N(CC)CC)C>[NH2:3][C:4]1[C:9]([F:10])=[CH:8][CH:7]=[C:6]([NH:13][C:14]([CH3:21])([CH3:20])[CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])[N:5]=1.[NH2:3][C:4]1[C:9]([F:10])=[C:8]([Br:11])[CH:7]=[C:6]([NH:13][C:14]([CH3:21])([CH3:20])[CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 887MethanolHCID 221211602-Amino-4-bromo-5-chloro-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine

生成物 2

HCID 177787632-Amino-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridineHCID 221212652-Amino-4-bromo-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 8471
Triethylamine
溶媒

実験手順

To 10 ml of methanol were added 1.6 g of 2-amino-4-bromo-5-chloro-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine together with 0.47 g of triethylamine and 0.09 g of 10% palladium on carbon, and the mixture was hydrogenated at room temperature for 39 hours. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 50 ml of chloroform, and the mixture was washed with 50 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to chromatography (silica gel, 25 g; eluent: chloroform) to obtain 0.75 g of 2-amino-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine as a pale brown oil, and 0.2 g of 2-amino-4-bromo-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine 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 50 ml of chloroform
  4. washthe mixture was washed with 50 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-9cf5056e24b144a98f8cc533fa3959e4
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06133284

反応ノート

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