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

HRID 627720노트

반응식

HRID 627720 반응식
[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

참가 물질

3

반응물 1

HCID 867281553-Nitro-5-(trifluoromethyl)picolinamide

생성물 1

HCID 867281563-Amino-5-(trifluoromethyl)picolinamide수율 97%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-35eb8daf8fd0461188c01d3cf7f12c9d
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309263B2

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