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

HRID 1742065노트

반응식

HRID 1742065 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-40c90b2901424f54aa045690bb3adc26
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05336780

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