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

HRID 251922

반응식

HRID 251922 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 13167844N-(2-methylaminobenzoyl)-N'-ethoxycarbonylhydrazine수율 50.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-4dee796b6fc0461ab963238e1978c11e
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867949B2

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