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

HRID 59611

反応式

HRID 59611 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>[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

5

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 1

HCID 176Acetic Acid溶媒

実験手順

A solution of ethyl-2-[(3-bromo-2-methoxyphenyl)hydrazono]-3-oxobutanoate (5 g) prepared as in Example 1, and 3,4-dimethylphenylhydrazine hydrochloride (2.48 g) and sodium acetate (1.4 g) in glacial acetic acid (100 mL) was stirred and heated to reflux for about 3 hours. The mixture was cooled to about room temperature and stirred for about 1 hour. It was filtered, washed with water (25 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours to obtain an orange solid product. Yield: 4.15 g; Melting point: 197.4-198.2° C.; Purity (HPLC): 99.33%

後処理

  1. temperatureheated
  2. temperatureto reflux for about 3 hours
  3. temperatureThe mixture was cooled to about room temperature
  4. stirringstirred for about 1 hour
  5. filtrationIt was filtered
  6. washwashed with water (25 mL)
  7. customdried in an oven at about 55° C. to about 60° C. for about 12 hours
  8. customto obtain an orange solid product

出典と根拠

ORDレコード
ord-82ebaf342c6448da820299c8ce483664
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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