3-Nitro-5-(trifluoromethyl)picolinamide → 3-Amino-5-(trifluoromethyl)picolinamide

HRID 627720ノート

反応式

HRID 627720 の反応式
[N+:1]([C:4]1[C:5]([C:14]([NH2:16])=[O:15])=[N:6][CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1)([O-])=O>[Pd]>[NH2:1][C:4]1[C:5]([C:14]([NH2:16])=[O:15])=[N:6][CH:7]=[C:8]([C:10]([F:13])([F:11])[F:12])[CH:9]=1

参加物

3

反応物 1

HCID 867281553-Nitro-5-(trifluoromethyl)picolinamide

生成物 1

HCID 867281563-Amino-5-(trifluoromethyl)picolinamide収率 97%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

A round bottom flask was charged with 3-nitro-5-(trifluoromethyl)picolinamide (850 mg, 3.62 mmol) and wet 5 wt. % Pd/C (769 mg, 0.362 mmol) and was purged with nitrogen. EtOAc (7230 μl) and then MeOH (7230 μl) were added, and the flask was evacuated and filled with hydrogen. The reaction was stirred at RT under hydrogen atmosphere for 17 h. The mixture was filtered through Celite and washed with EtOAc and MeOH. The filtrate was concentrated to provide 3-amino-5-(trifluoromethyl)picolinamide (720 mg, 3.51 mmol, 97% yield) as a white solid. LC/MS (ESI+) m/z=206.1 (M+H).

後処理

  1. customwas purged with nitrogen
  2. additionEtOAc (7230 μl) and then MeOH (7230 μl) were added
  3. customthe flask was evacuated
  4. additionfilled with hydrogen
  5. filtrationThe mixture was filtered through Celite
  6. washwashed with EtOAc and MeOH
  7. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-35eb8daf8fd0461188c01d3cf7f12c9d
出典データセット
uspto-grants-2016_04
特許番号
US09309263B2

反応ノート

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