Acetic Acid → HCID 19080735、化合物

HRID 963165ノート

反応式

HRID 963165 の反応式
C[O-].[Na+].CO.[CH2:6]([N:8]1[C:12]([CH3:13])=[C:11]([NH:14][S:15]([C:18]2[N:28]=[C:21]3[CH:22]=[C:23]([CH3:27])[CH:24]=[C:25](Cl)[N:20]3[N:19]=2)(=[O:17])=[O:16])[C:10]([C:29]([F:32])([F:31])[F:30])=[N:9]1)[CH3:7].[C:33](O)(=[O:35])C>CS(C)=O>[CH2:6]([N:8]1[C:12]([CH3:13])=[C:11]([NH:14][S:15]([C:18]2[N:28]=[C:21]3[CH:22]=[C:23]([CH3:27])[CH:24]=[C:25]([O:35][CH3:33])[N:20]3[N:19]=2)(=[O:17])=[O:16])[C:10]([C:29]([F:32])([F:31])[F:30])=[N:9]1)[CH3:7]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 887MethanolHCID 10942334Sodium MethoxideHCID 19080766HCID 19080766、化合物

生成物 1

HCID 19080735HCID 19080735、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A 25 percent solution of sodium methoxide in methanol (1.65 g, 5.4 mmol) was added to a solution of 1.14 g (2.70 mmol) of N-(1-ethyl-5-methyl-3-(trifluoromethyl)-4-pyrazolyl)-5-chloro-7-methyl[1,2,4]triazolo[1,5-a]pyridine-2-sulfonamide in 25 mL of dimethyl sulfoxide (DMSO) at ambient temperature with stirring. After 18 hours, 1.0 mL of acetic acid was added and the resulting mixture was concentrated by evaporation under reduced pressure. The residue was diluted with 25 mL of water and the resulting slurry was stirred for 10 min and then the insoluble solids collected by filtration, washed twice with 10 mL portions of water and then with 25 mL of ether, and dried under reduced pressure at 40° C. overnight. The resulting white solid, which amounted to 1.03 g (92 percent of theory) and melted at 230°-231° C. (d), was the title compound (Compound 2).

後処理

  1. concentrationthe resulting mixture was concentrated by evaporation under reduced pressure
  2. additionThe residue was diluted with 25 mL of water
  3. stirringthe resulting slurry was stirred for 10 min
  4. filtrationthe insoluble solids collected by filtration
  5. washwashed twice with 10 mL portions of water
  6. dry with materialwith 25 mL of ether, and dried under reduced pressure at 40° C. overnight

出典と根拠

ORDレコード
ord-a65dbfb3a46146729f0f63949949ec2e
出典データセット
uspto-grants-1998_06
特許番号
US05763359

反応ノート

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