1-(3,4-Dimethylphenyl)hydrazine hydrochloride → 4-[(3-bromo-2-methoxyphenyl)hydrazinylidene]-2-(3,4-dimethylphenyl)-5-methylpyrazol-3-one

HRID 59625

反応式

HRID 59625 の反応式
C(O[C:4](=[O:20])[C:5](=[N:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([Br:17])[C:12]=1[O:18][CH3:19])[C:6](=O)[CH3:7])C.Cl.[CH3:22][C:23]1[CH:24]=[C:25]([NH:30][NH2:31])[CH:26]=[CH:27][C:28]=1[CH3:29].C([O-])(=O)C.[Na+]>C(O)(=O)C.O>[CH3:22][C:23]1[CH:24]=[C:25]([N:30]2[C:4](=[O:20])[C:5](=[N:9][NH:10][C:11]3[CH:16]=[CH:15][CH:14]=[C:13]([Br:17])[C:12]=3[O:18][CH3:19])[C:6]([CH3:7])=[N:31]2)[CH:26]=[CH:27][C:28]=1[CH3:29]

参加物

6

反応物 3

HCID 1737401-(3,4-Dimethylphenyl)hydrazine hydrochlorideHCID 517045Sodium AcetateHCID 178472845HCID 178472845、化合物

生成物 1

HCID 1784863784-[(3-bromo-2-methoxyphenyl)hydrazinylidene]-2-(3,4-dimethylphenyl)-5-methylpyrazol-3-one

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

A solution of ethyl-2-[(3-bromo-2-methoxyphenyl)hydrazono]-3-oxobutanoate (10 g) prepared as in Example 15, and 3,4-dimethylphenylhydrazine hydrochloride (6.05 g) and sodium acetate (2.63 g) in acetic acid (150 mL) was stirred and heated to about 80° C. to about 90° C. for about 3 hours. The reaction mixture was cooled to about room temperature and stirred for about 1 hour. The reaction mixture was filtered to give a solid, which was washed with acetic acid. The solid obtained was stirred in water for about 30 minutes at about room temperature, which was then filtered, washed with water and dried at about 55° C. to about 60° C. Yield: 11 g

後処理

  1. temperatureheated to about 80° C. to about 90° C. for about 3 hours
  2. temperatureThe reaction mixture was cooled to about room temperature
  3. stirringstirred for about 1 hour
  4. filtrationThe reaction mixture was filtered
  5. customto give a solid, which
  6. washwas washed with acetic acid
  7. customThe solid obtained
  8. filtrationwhich was then filtered
  9. washwashed with water
  10. customdried at about 55° C. to about 60° C

出典と根拠

ORDレコード
ord-1056531128df4c94bfd4e1c666651145
出典データセット
uspto-grants-2016_09
特許番号
US09440927B2

関連ノート

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