Acetic Acid → HCID 21464438, 화합물

HRID 1898811노트

반응식

HRID 1898811 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:29]=[C:21]2[CH:22]=[C:23](Cl)[CH:24]=[C:25]([O:26][CH3:27])[N:20]2[N:19]=1)(=[O:17])=[O:16].[C:30](O)(=[O:32])C>CS(C)=O.ClCCl>[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:29]=[C:21]2[CH:22]=[C:23]([O:32][CH3:30])[CH:24]=[C:25]([O:26][CH3:27])[N:20]2[N:19]=1)(=[O:17])=[O:16]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 10942334Sodium MethoxideHCID 21464355HCID 21464355, 화합물

생성물 1

HCID 21464438HCID 21464438, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6344Dichloromethane용매

실험 절차

Sodium methoxide in methanol (3.0 mL of 25 percent solution, 0.71 g, 0.013 mol) was added to a solution of N-(2,6-dichlorophenyl)-5-methoxy-7-chloro[1,2,4]triazolo[1,5-a]pyridine-2-sulfonamide (0.66 g, 0.0016 mol) in dimethyl sulfoxide (30 mL) with stirring over several hours. The mixture was allowed to react and 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 chromatographed on silica gel starting with 0.5 percent acetic acid in dichloromethane and gradually increasing the strength to 0.5 percent acetic acid plus 1.0 percent ethanol in dichloromethane. The product fractions were concentrated by evaporation under reduced pressure to obtain 118 mg (13 percent of theory) of the title compound as a pale yellow powder melting at 252°-253° C.(d).

후처리

  1. customto react
  2. customThe resulting organic phase was recovered
  3. washwashed with water
  4. customthe volatiles were removed by evaporation under reduced pressure
  5. customThe residue obtained
  6. customwas chromatographed on silica gel starting with 0.5 percent acetic acid in dichloromethane
  7. temperaturegradually increasing the strength to 0.5 percent acetic acid plus 1.0 percent ethanol in dichloromethane
  8. concentrationThe product fractions were concentrated by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-f1138f1804164c72bed7d33b44dd1943
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05571775

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