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

HRID 1793080

반응식

HRID 1793080 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-07a7055c4d7c49e6ac9330386c5fda72
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07078405B2

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