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

HRID 1526638ノート

反応式

HRID 1526638 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 (72300 and then MeOH (72300 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 (72300 and then MeOH (72300 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-1a69262c1a5f4a64a08315a5bc276c0b
出典データセット
uspto-grants-2015_07
特許番号
US09085576B2

反応ノート

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