Acetic Acid → HCID 19080735, 화합물

HRID 963165노트

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HRID 963165 반응식
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]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 10942334Sodium MethoxideHCID 19080766HCID 19080766, 화합물

생성물 1

HCID 19080735HCID 19080735, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a65dbfb3a46146729f0f63949949ec2e
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763359

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