Hydrochloric Acid → 1-Acetyl-6-methyl-3-(3-nitro-phenyl)pyrazolo[5,1-c][1,2,4]triazole

HRID 1742065ノート

反応式

HRID 1742065 の反応式
[C:1]([NH:4][C:5]1[N:9]([C:10](=[N:20]OS(C2C=CC(C)=CC=2)(=O)=O)[C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=2)[N:8]=[C:7]([CH3:32])[CH:6]=1)(=[O:3])[CH3:2].C1CCN2C(=NCCC2)CC1.Cl>CS(C)=O.O>[C:1]([N:4]1[C:5]2=[CH:6][C:7]([CH3:32])=[N:8][N:9]2[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=2)=[N:20]1)(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 735084175-acetamido-3-methyl-1-(O-tosyl-3-nitro-benzohydroximoyl)-pyrazole

生成物 1

HCID 190101071-Acetyl-6-methyl-3-(3-nitro-phenyl)pyrazolo[5,1-c][1,2,4]triazole収率 90.1%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

800 mg (1.75 mmol) of 5-acetamido-3-methyl-1-(O-tosyl-3-nitro-benzohydroximoyl)-pyrazole are suspended in 10 ml of DMSO, treated with 0.8 ml DBU with stirring at room temperature, diluted with water and acidified with 2N hydrochloric acid. The precipitate obtained is filtered under suction, washed with water, a little methanol and a little ethyl acetate and recrystallised from methyl glycol. 450 mg (90%) of 1-acetyl-6-methyl-3-(3-nitro-phenyl)pyrazolo[5,1-c][1,2,4]triazole with a m. pt. of 207°-210° C. are obtained.

後処理

  1. customThe precipitate obtained
  2. filtrationis filtered under suction
  3. washwashed with water
  4. customa little methanol and a little ethyl acetate and recrystallised from methyl glycol

出典と根拠

ORDレコード
ord-40c90b2901424f54aa045690bb3adc26
出典データセット
uspto-grants-1994_08
特許番号
US05336780

反応ノート

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