Acetic Acid → HCID 21464355, 화합물

HRID 1940902노트

반응식

HRID 1940902 반응식
C[O-].[Na+].CO.[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=1[NH:14][S:15]([C:18]1[N:28]=[C:21]2[CH:22]=[C:23]([Cl:27])[CH:24]=[C:25](Cl)[N:20]2[N:19]=1)(=[O:17])=[O:16].[C:29](O)(=[O:31])C>CS(C)=O.ClCCl.CCCCCC>[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=1[NH:14][S:15]([C:18]1[N:28]=[C:21]2[CH:22]=[C:23]([Cl:27])[CH:24]=[C:25]([O:31][CH3:29])[N:20]2[N:19]=1)(=[O:17])=[O:16]

참가 물질

8

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 10942334Sodium MethoxideHCID 21464351HCID 21464351, 화합물

생성물 1

HCID 21464355HCID 21464355, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 6344Dichloromethane용매HCID 8058Hexane용매

실험 절차

Sodium methoxide in methanol (1.1 mL of 25 percent solution, 0.26 g, 0.005 mol) was added to a solution of N-(2,6-dichlorophenyl)-5,7-dichloro[1,2,4]triazolo[1,5-a]pyridine-2-sulfonamide (0.9 g, 0.02 mol) in dimethyl sulfoxide (30 mL) at ambient temperature with stirring. The reaction was complete in a few minutes, but was stirred for 30 min. The mixture was then acidified with acetic acid and diluted with dichloromethane. The resulting organic phase was recovered and washed with water and the volatiles were removed by evaporation under reduced pressure. The residue obtained was mixed with hexane and the insoluble solids were collected by filtration and dried to obtain 0.8 g (90 percent of theory) of the title compound as a light tan powder melting at 232°-234° C.(d).

후처리

  1. waitThe reaction was complete in a few minutes
  2. stirringwas stirred for 30 min
  3. customThe resulting organic phase was recovered
  4. washwashed with water
  5. customthe volatiles were removed by evaporation under reduced pressure
  6. customThe residue obtained
  7. filtrationthe insoluble solids were collected by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-f6e16fb264ca4bb29ffc1703c42cb6f9
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700940

반응 노트

불러오는 중…