Potassium Carbonate → N-(2-methoxycarbonylphenylsulfonyl)-1,5-dimethylpyrazole-3-carboxamide

HRID 1655887

反応式

HRID 1655887 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11]([NH2:14])(=[O:13])=[O:12])=[O:4].[CH3:15][N:16]1[C:20]([CH3:21])=[CH:19][C:18]([C:22](Cl)=[O:23])=[N:17]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:1][O:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11]([NH:14][C:22]([C:18]1[CH:19]=[C:20]([CH3:21])[N:16]([CH3:15])[N:17]=1)=[O:23])(=[O:13])=[O:12])=[O:4]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 42546Benzoic acid, 2-(aminosulfonyl)-, methyl esterHCID 27763641,5-Dimethyl-1H-Pyrazole-3-Carbonyl Chloride

生成物 1

HCID 19789275N-(2-methoxycarbonylphenylsulfonyl)-1,5-dimethylpyrazole-3-carboxamide収率 68.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

10.8 g of 2-methoxycarbonylphenylsulfonamide, 8.6 g of 1,5-dimethylpyrazole-3-carbonyl chloride and 13.8 g of potassium carbonate in 200 ml of absolute acetone are refluxed for 8 h. The solvent is removed by distillation and then the residue is taken up in water and the pH is adjusted to 2. The precipitate is filtered off with suction and washed with H2O until neutral. The residue is stirred with ether, filtered off with suction and dried under reduced pressure. 11.6 g of N-(2-methoxycarbonylphenylsulfonyl)-1,5-dimethylpyrazole-3-carboxamide with a melting point of 176°-177° C. are obtained (active ingredient Example No. 40).

後処理

  1. customThe solvent is removed by distillation
  2. filtrationThe precipitate is filtered off with suction
  3. washwashed with H2O until neutral
  4. filtrationfiltered off with suction
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-e5e328d007e548d3853bd9f38157dfaa
出典データセット
uspto-grants-1993_10
特許番号
US05252540

関連ノート

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