Pyridine → N-(2,6-Dichloro-3-methylphenyl)-5-formylamino-1,2,4-triazole-5-sulfonamide

HRID 275040

反応式

HRID 275040 の反応式
[Cl:1][C:2]1[C:8]([CH3:9])=[CH:7][CH:6]=[C:5]([Cl:10])[C:3]=1[NH2:4].C(N[C:14]1[NH:18][N:17]=[C:16]([S:19](Cl)(=[O:21])=[O:20])[N:15]=1)=O.[OH-:23].[Na+].C(Cl)(Cl)Cl.[N:29]1[CH:34]=CC=CC=1>>[Cl:1][C:2]1[C:8]([CH3:9])=[CH:7][CH:6]=[C:5]([Cl:10])[C:3]=1[NH:4][S:19]([C:16]1([NH:29][CH:34]=[O:23])[N:17]=[N:18][CH:14]=[N:15]1)(=[O:20])=[O:21]

参加物

6

反応物 5

HCID 1049PyridineHCID 6212ChloroformHCID 14798Sodium HydroxideHCID 1165292,6-Dichloro-3-methylanilineHCID 178522608HCID 178522608、化合物

生成物 1

HCID 20077588N-(2,6-Dichloro-3-methylphenyl)-5-formylamino-1,2,4-triazole-5-sulfonamide

反応条件

温度
70 °C

実験手順

To a mixture of 1 g (5.2 mmol) of 2,6-dichloro-3-methylaniline in 2 ml pyridine was added 1 g (4.7 mmol) of 5-formylamino-3-chlorosulfonyl-1,2,4-triazole over a period of 5 minutes. The mixture was heated with stirring to 70° C. for 4 hours. It was then cooled and dispersed between 25 ml of 1N aqueous sodium hydroxide and 50 ml of chloroform. The aqueous layer was recovered, extracted with more chloroform, and acidified with aqueous hydrochloric acid. The solids that formed were collected by filtration and dried to obtain 1.0 g (59 percent of theory) of the title compound, m.p. 275°-279° C. The infrared and carbon nmr spectra were consistent with the assigned structure.

後処理

  1. temperatureThe mixture was heated
  2. temperatureIt was then cooled
  3. customThe aqueous layer was recovered
  4. extractionextracted with more chloroform
  5. customThe solids that formed
  6. filtrationwere collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-a0fb4fe0214d4f7e9cc372b0d6acbc71
出典データセット
uspto-grants-1995_02
特許番号
US05391759

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