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

HRID 1742062ノート

反応式

HRID 1742062 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9951e2f903c54e1da04e592485a75fc4
出典データセット
uspto-grants-1994_08
特許番号
US05336780

反応ノート

読み込み中…