Ethanol → N-(2-methylaminobenzoyl)-N'-ethoxycarbonylhydrazine

HRID 251922

反応式

HRID 251922 の反応式
C[N:2]1[C:8](=O)[O:7][C:5](=O)[C:4]2=[CH:10][CH:11]=[CH:12][CH:13]=[C:3]12.[C:14]([O:18][CH2:19][CH3:20])(=[O:17])[NH:15][NH2:16].C(O)C>C(OCC)(=O)C>[CH3:8][NH:2][C:3]1[CH:13]=[CH:12][CH:11]=[CH:10][C:4]=1[C:5]([NH:16][NH:15][C:14]([O:18][CH2:19][CH3:20])=[O:17])=[O:7]

参加物

5

反応物 3

HCID 702EthanolHCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 25160N-Methylisatoic anhydride

生成物 1

HCID 13167844N-(2-methylaminobenzoyl)-N'-ethoxycarbonylhydrazine収率 50.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 8.86 g of N-methylisatoic anhydride, 5.73 g of ethyl carbazate and 25 ml of ethanol was heated to reflux for 2 hours. After the reaction mixture was allowed to around room temperature, ethyl acetate was added thereto and the mixture was washed with water two times. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was washed with methyl tert-butyl ether to obtain 5.99 g of N-(2-methylaminobenzoyl)-N′-ethoxycarbonylhydrazine of the formula:

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. customwas allowed to around room temperature
  4. washthe mixture was washed with water two times
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. washThe resulting residue was washed with methyl tert-butyl ether

出典と根拠

ORDレコード
ord-4dee796b6fc0461ab963238e1978c11e
出典データセット
uspto-grants-2011_01
特許番号
US07867949B2

関連ノート

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