Acetic Acid → HCID 21464355、化合物

HRID 1940902ノート

反応式

HRID 1940902 の反応式
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]

参加物

8

反応物 4

HCID 176Acetic AcidHCID 887MethanolHCID 10942334Sodium MethoxideHCID 21464351HCID 21464351、化合物

生成物 1

HCID 21464355HCID 21464355、化合物

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 6344Dichloromethane溶媒HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f6e16fb264ca4bb29ffc1703c42cb6f9
出典データセット
uspto-grants-1997_12
特許番号
US05700940

反応ノート

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