Methanol → N-(2-amino-5-chloro-3-methylbenzoyl)-N'-methoxycarbonylhydrazine

HRID 251925노트

반응식

HRID 251925 반응식
[Cl:1][C:2]1[CH:13]=[C:12]([CH3:14])[C:5]2[NH:6]C(=O)O[C:9](=[O:10])[C:4]=2[CH:3]=1.[C:15]([O:19][CH3:20])(=[O:18])[NH:16][NH2:17].CO>O>[NH2:6][C:5]1[C:12]([CH3:14])=[CH:13][C:2]([Cl:1])=[CH:3][C:4]=1[C:9]([NH:17][NH:16][C:15]([O:19][CH3:20])=[O:18])=[O:10]

참가 물질

5

반응물 3

HCID 887MethanolHCID 80519Methyl carbazateHCID 115502595-Chloro-3-methyl isatoic anhydride

생성물 1

HCID 66854326N-(2-amino-5-chloro-3-methylbenzoyl)-N'-methoxycarbonylhydrazine수율 60.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.05 g of 6-chloro-8-methyl-1H-benzo[d]-1,3-oxazine-2,4-dione, 0.46 g of methyl carbazate and 20 ml of methanol was heated to reflux for 3 hours. After the reaction mixture was allowed to cool to around room temperature, water was poured thereto and the mixture was extracted with ethyl acetate three times. The resulting organic layer was concentrated under reduced pressure, and the residue was washed with toluene to obtain 0.77 g of N-(2-amino-5-chloro-3-methylbenzoyl)-N′-methoxycarbonylhydrazine of the formula:

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 3 hours
  3. temperatureto cool to around room temperature
  4. extractionthe mixture was extracted with ethyl acetate three times
  5. concentrationThe resulting organic layer was concentrated under reduced pressure
  6. washthe residue was washed with toluene

출처 및 근거

ORD 기록
ord-edb1e9fb023140cda37768f2d9730a17
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867949B2

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