Triethylamine → 5-Amino-1-(3-nitro-benzohydroximoyl)-3-methyl-pyrazole

HRID 1742062노트

반응식

HRID 1742062 반응식
[CH3:1][C:2]1[NH:6][N:5]=[C:4]([NH2:7])[CH:3]=1.C(N(CC)CC)C.[N+:15]([C:18]1[CH:19]=[C:20]([CH:25]=[CH:26][CH:27]=1)[C:21](Cl)=[N:22][OH:23])([O-:17])=[O:16]>O1CCOCC1>[NH2:7][C:4]1[N:5]([C:21](=[N:22][OH:23])[C:20]2[CH:25]=[CH:26][CH:27]=[C:18]([N+:15]([O-:17])=[O:16])[CH:19]=2)[N:6]=[C:2]([CH3:1])[CH:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 2756318alpha-Chloro-3-nitrobenzaldoxime

생성물 1

HCID 735084165-Amino-1-(3-nitro-benzohydroximoyl)-3-methyl-pyrazole수율 75%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

4.85 g (0.05 mol) of 3(5)-amino-5(3)-methyl-pyrazole in 50 ml of absolute dioxan are treated with 8.3 ml (0,06 mol) of triethylamine and then, under stirring at room temperature, are treated dropwise with a solution of 10 g (0.05 mol) of 3-nitro-benzohydroximoyl chloride in 50 ml of absolute dioxan. Stirring is continued for 3 hours and then the mixture is evaporated to dryness. The residue is treated with water and ethyl acetate. The organic phase is dried over magnesium sulphate, evaporated under vacuum and the residue obtained in this way is recrystallised from dioxan. 9.8 g (48%) of 5-amino-1-(3-nitro-benzohydroximoyl)-3-methyl-pyrazole with a m. pt. of 224° to 226° C. are obtained.

후처리

  1. stirringStirring
  2. customthe mixture is evaporated to dryness
  3. additionThe residue is treated with water and ethyl acetate
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. customevaporated under vacuum
  6. customthe residue obtained in this way
  7. customis recrystallised from dioxan

출처 및 근거

ORD 기록
ord-9951e2f903c54e1da04e592485a75fc4
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05336780

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