Ammonium formate → 4-(4-Methoxy-2-methylphenyl)-3-pyridazineamine

HRID 501003

반응식

HRID 501003 반응식
C([O-])=O.[NH4+].Cl[C:6]1[N:11]=[N:10][C:9]([NH2:12])=[C:8]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=2[CH3:21])[CH:7]=1>CO.[Pd]>[CH3:20][O:19][C:16]1[CH:17]=[CH:18][C:13]([C:8]2[CH:7]=[CH:6][N:11]=[N:10][C:9]=2[NH2:12])=[C:14]([CH3:21])[CH:15]=1

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 220244746-Chloro-4-(4-methoxy-2-methylphenyl)-3-pyridazineamine

생성물 1

HCID 220244894-(4-Methoxy-2-methylphenyl)-3-pyridazineamine수율 90.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

10% Pd—C (hydrous product; 7.89 g) and ammonium formate (11.96 g) were added to a solution of 6-chloro-4-(4-methoxy-2-methylphenyl)-3-pyridazineamine (7.89 g) in methanol (100 mL), and the mixture was heated under reflux for 1.5 hours. The reaction mixture was filtered through Celite, and the solvent was evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate:ethanol=10:1) to give the title compound (6.16 g) as white crystals.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. filtrationThe reaction mixture was filtered through Celite
  4. customthe solvent was evaporated
  5. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:ethanol=10:1)

출처 및 근거

ORD 기록
ord-864c31f1255244eab1b56df523273f4a
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772249B2

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