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Hydrochloric Acid → 2-Amino-6-(t-butylamino)-5-fluoropyridine

HRID 368446
ノート
印刷プレビュー

反応式

HRID 368446 の反応式
Cl.C([NH:9][C:10]1[C:15]([Cl:16])=[CH:14][C:13]([F:17])=[C:12]([NH:18][C:19]([CH3:22])([CH3:21])[CH3:20])[N:11]=1)C1C=CC=CC=1>[Pd].CO>[NH2:9][C:10]1[C:15]([Cl:16])=[CH:14][C:13]([F:17])=[C:12]([NH:18][C:19]([CH3:22])([CH3:21])[CH3:20])[N:11]=1.[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:17])=[C:12]([NH:18][C:19]([CH3:22])([CH3:21])[CH3:20])[N:11]=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 313Hydrochloric AcidHCID 221211832-Benzylamino-6-(t-butylamino)-3-chloro-5-fluoropyridine

生成物 2

HCID 221212302-Amino-6-(t-butylamino)-5-fluoropyridineHCID 221212492-Amino-6-(t-butylamino)-3-chloro-5-fluoropyridine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol
溶媒

実験手順

To a mixed solution of 18 ml methanol and 1.4 g concentrated hydrochloric acid were added 3.1 g of 20 2-benzylamino-6-(t-butylamino)-3-chloro-5-fluoropyridine together with 0.33 g of 10% palladium on carbon, and the mixture was hydrogenated at 30° C. for 1 hour. 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 10 ml of 6% aqueous solution of sodium hydroxide, and the chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to column chromatography (silica gel, 40 g; eluent: chloroform:n-hexane, 3:1 and then 1:1) to obtain 1.35 g of 2-amino-6-(t-butylamino)-3-chloro-5-fluoropyridine as a pale brown oil, and 0.32 g of 2-amino-6-(t-butylamino)-5-fluoropyridine 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 10 ml of 6% aqueous solution of sodium hydroxide
  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-0850b0360d504aeab40dc6e2526bb79c
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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