Triethylamine → N-(3,5-dimethylisoxazol-4-yl)-3-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide

HRID 1607231

반응식

HRID 1607231 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:13]([C:15]([O:17][CH3:18])=[O:16])([CH3:14])[CH2:12][NH:11][N:10]=2)=[CH:5][CH:4]=1.C(N(CC)CC)C.[CH3:26][C:27]1[C:31]([N:32]=[C:33]=[O:34])=[C:30]([CH3:35])[O:29][N:28]=1>C(Cl)Cl>[CH3:26][C:27]1[C:31]([NH:32][C:33]([N:11]2[CH2:12][C:13]([C:15]([O:17][CH3:18])=[O:16])([CH3:14])[C:9]([C:6]3[CH:5]=[CH:4][C:3]([Cl:2])=[CH:8][CH:7]=3)=[N:10]2)=[O:34])=[C:30]([CH3:35])[O:29][N:28]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27362663,5-Dimethylisoxazole-4-isocyanateHCID 198521223-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole hydrochloride

생성물 1

HCID 19852785N-(3,5-dimethylisoxazol-4-yl)-3-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole hydrochloride (10 mmole), triethylamine (20 mmole), methylene chloride (30 ml and 3,5-dimethylisoxazole-4-yl isocyanate (Maybridge Chemical Co. Ltd.) (10 mmole) were reacted by stirring at room temperature for 30 minutes. The reaction mixture was then washed twice with water, dried with magnesium sulfate concentrated giving a 95% yield of N-(3,5-dimethylisoxazol-4-yl)-3-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide mp 214°-216° C. NMR data was consistent with the structure.

후처리

  1. washThe reaction mixture was then washed twice with water
  2. dry with materialdried with magnesium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-163a787293e64610890665b1deaaa9f7
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863947

연결된 노트

불러오는 중…