Hydrochloric Acid → 2-(4-Aminophenyl)-5-methyl-2,4-dihydro-3H-pyrazol-3-one dihydrochloride

HRID 1722728

반응식

HRID 1722728 반응식
[CH3:1][C:2]1[CH2:6][C:5](=[O:7])[N:4]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=2)[N:3]=1.[ClH:17]>[Pd].CO>[ClH:17].[ClH:17].[NH2:14][C:11]1[CH:10]=[CH:9][C:8]([N:4]2[C:5](=[O:7])[CH2:6][C:2]([CH3:1])=[N:3]2)=[CH:13][CH:12]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 808163H-Pyrazol-3-one, 2,4-dihydro-5-methyl-2-(4-nitrophenyl)-

생성물 1

HCID 125543512-(4-Aminophenyl)-5-methyl-2,4-dihydro-3H-pyrazol-3-one dihydrochloride수율 68%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Into 310 ml of methanol, 500 mg of 3-methyl-1-(4-nitrophenyl)-2-pyrazolin-5-one was dissolved, 50 mg of 5% Pd/C and 0.6 ml of conc. hydrochloric acid were added to the solution, and the mixture was stirred under hydrogen atmosphere to consume the calculated amount of hydrogen. Then, the catalyst was filtered off and the filtrate was concentrated. The residue was recrystallized from methanol-ethyl ether to give 409 mg of 1-(4-aminophenyl)-3-methyl-2-pyrazolin-5-one dihydrochloride (Compound No. 50) as pale brown crystals.

후처리

  1. customto consume the calculated amount of hydrogen
  2. filtrationThen, the catalyst was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe residue was recrystallized from methanol-ethyl ether

출처 및 근거

ORD 기록
ord-aa74edaeba974b96889e35ec8724ef24
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04857542

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