p-Nitroacetophenone → 3-(4-Nitrophenyl)-1H-pyrazole

HRID 1251466

反応式

HRID 1251466 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][CH:5]=1)=O.COC(OC)[N:16]([CH3:18])C.[NH2:21]N>O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[N+:10]([C:7]1[CH:8]=[CH:9][C:4]([C:2]2[NH:21][N:16]=[CH:18][CH:1]=2)=[CH:5][CH:6]=1)([O-:12])=[O:11]

参加物

5

反応物 3

HCID 7487p-NitroacetophenoneHCID 9321HydrazineHCID 78373Dimethylformamide dimethyl acetal

生成物 1

HCID 27370713-(4-Nitrophenyl)-1H-pyrazole収率 58.8%

試薬・触媒・溶媒 1

HCID 521998p-Toluenesulfonic acid monohydrate触媒

実験手順

4-Nitroacetophenone(15 g) and N,N-dimethylformamide dimethylacetal(54 g) were refluxed for 1 hour. The reaction mixture was cooled, then crystals precipitate were filtered. To a solution of the crystals obtained (13.5 g) in ethanol (150 ml) was added hydrazine (4.52 g) and p-toluene sulfonic acid monohydrate (0.15 g) and the mixture was refluxed for 1 hours. The solvent was evaporated to dryness and the residue was crystallized from ether to obtain thr title compound (10.1 g).

後処理

  1. temperatureThe reaction mixture was cooled
  2. filtrationcrystals precipitate were filtered
  3. customTo a solution of the crystals obtained (13.5 g) in ethanol (150 ml)
  4. temperaturethe mixture was refluxed for 1 hours
  5. customThe solvent was evaporated to dryness
  6. customthe residue was crystallized from ether

出典と根拠

ORDレコード
ord-743f2d07680d45fe878525b9a98c2a9b
出典データセット
uspto-grants-2002_01
特許番号
US06342516B1

関連ノート

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