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

HRID 1607228ノート

反応式

HRID 1607228 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e2c2c168c6e64ba5af9d5fef24427ded
出典データセット
uspto-grants-1989_09
特許番号
US04863947

反応ノート

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