4-Nitrobenzamidine hydrochloride → HCID 67295444, 화합물

HRID 629031

반응식

HRID 629031 반응식
O(C)[Na].[CH3:4][O:5][CH:6]([C:12]([O:14]C)=O)[C:7]([O:9]CC)=O.Cl.[N+:17]([C:20]1[CH:28]=[CH:27][C:23]([C:24](=[NH:26])[NH2:25])=[CH:22][CH:21]=1)([O-:19])=[O:18]>CCO>[OH:14][C:12]1[N:25]=[C:24]([C:23]2[CH:22]=[CH:21][C:20]([N+:17]([O-:19])=[O:18])=[CH:28][CH:27]=2)[NH:26][C:7](=[O:9])[C:6]=1[O:5][CH3:4]

참가 물질

5

반응물 3

HCID 1706254-Nitrobenzamidine hydrochlorideHCID 57351026Ethyl methyl methoxypropanedioateHCID 178418582HCID 178418582, 화합물

생성물 1

HCID 67295444HCID 67295444, 화합물수율 65%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

The NaOCH3 (7.8 g, 3 eq) was added to a stirred solution of 1-ethyl 3-methyl 2-methoxymalonate (11 g, 1.3 eq), 4-nitrobenzimidamide hydrochloride (9.6 g, 1 eq) and EtOH (240 ml) and the mixture was refluxed for 8 hrs. After 8 hrs, the solvent was evaporated and water (10˜15 ml) was added to the mixture then the mixture was cooled to 0° C. and carefully acidified with conc. HCl. After overnight cooling, it led to the formation of brown precipitates. The mixture was filtered and the precipitates was dried in vacuo to give a brown solid (65%) as a product.

후처리

  1. temperaturethe mixture was refluxed for 8 hrs
  2. customthe solvent was evaporated
  3. additionwater (10˜15 ml) was added to the mixture
  4. temperatureAfter overnight cooling
  5. filtrationThe mixture was filtered
  6. customthe precipitates was dried in vacuo

출처 및 근거

ORD 기록
ord-89b00234122243398bfec657cbefe635
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315491B2

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