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

HRID 1655887

반응식

HRID 1655887 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e5e328d007e548d3853bd9f38157dfaa
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05252540

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