Triethylamine → Methyl 3-(4-chlorophenyl)-4,5-dihydro-4-methyl-1-(((4-(trifluoromethyl)phenyl)amino)carbonyl)-1H-pyrazole-4-carboxylate

HRID 1607228노트

반응식

HRID 1607228 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.[F:26][C:27]([F:38])([F:37])[C:28]1[CH:33]=[CH:32][C:31]([N:34]=[C:35]=[O:36])=[CH:30][CH:29]=1>C(Cl)Cl>[F:26][C:27]([F:37])([F:38])[C:28]1[CH:29]=[CH:30][C:31]([NH:34][C:35]([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:36])=[CH:32][CH:33]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 737684-(Trifluoromethyl)phenyl isocyanateHCID 198521223-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole hydrochloride

생성물 1

HCID 108039Methyl 3-(4-chlorophenyl)-4,5-dihydro-4-methyl-1-(((4-(trifluoromethyl)phenyl)amino)carbonyl)-1H-pyrazole-4-carboxylate수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole hydrochloride (Example P) (10 mmole), triethylamine (20 mmole), methylene chloride (30 ml) were added together and stirred for 10 minutes, whereon 10 mmole of 4-trifluoromethylphenyl isocyanate was added and after 30 minutes the resulting mixture was washed twice with water, dried with magnesium sulfate and concentrated giving a 95% yield of N-(4-trifluoromethylphenyl)-3-(4-chlorophenyl)-4-carbomethoxy-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide. NMR data was consistent with the structure.

후처리

  1. additionwas added and after 30 minutes the resulting mixture
  2. washwas washed twice with water
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e2c2c168c6e64ba5af9d5fef24427ded
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863947

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