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

HRID 1526638노트

반응식

HRID 1526638 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 (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).

후처리

  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

출처 및 근거

ORD 기록
ord-1a69262c1a5f4a64a08315a5bc276c0b
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085576B2

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