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

HRID 1290561

反応式

HRID 1290561 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c414a4f8e1d34e24a585075ee8f82241
出典データセット
uspto-grants-1998_05
特許番号
USRE035801

関連ノート

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