Hydrochloric Acid → HCID 53652618、化合物

HRID 128256

反応式

HRID 128256 の反応式
[Na+].[C:2]([C:5]1[S:9][C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[C:6]=1[S:14]([O-:17])(=O)=[O:15])(O)=[O:3].P(Cl)(Cl)(Cl)(Cl)[Cl:19].[ClH:24]>P(Cl)(Cl)(Cl)=O>[Cl:24][C:2]([C:5]1[S:9][C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[C:6]=1[S:14]([Cl:19])(=[O:17])=[O:15])=[O:3]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24819Phosphorus pentachlorideHCID 23714405Sodium 2-carboxy-benzo[b]thiophene-3-sulfonate

生成物 1

HCID 53652618HCID 53652618、化合物

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

反応条件

温度
100 °C

実験手順

44.0 gm (0.157 mol) of the above 2-carboxy-benzo[b]thiophene-3-sulfonic acid mono sodium salt were suspended in 200 cc of phosphorus oxychloride and admixed with 65.4 gm (0.314 mol) of phosphorus-(V)-chloride. To complete the reaction which was exothermic in the beginning accompanied by evolution of hydrogen chloride, the reaction mixture was heated to 100° C. for 2 hours, cooled and the inorganic salts were filtered off. After evaporation in vacuo, the residue was taken up in 300 cc of dry chloroform, the solution was filtered and again evaporated. The oily residue, consisting of 27 gm (58% of theory) of raw 2-chlorocarbonyl-benzo[b]thiophene-3-sulfonic acid chloride, crystallized upon cooling (m.p. 45°-47° C.) and was used without further purification in the next step.

後処理

  1. customthe reaction which
  2. temperaturecooled
  3. filtrationthe inorganic salts were filtered off
  4. customAfter evaporation in vacuo
  5. filtrationthe solution was filtered
  6. customagain evaporated
  7. customcrystallized
  8. temperatureupon cooling (m.p. 45°-47° C.)
  9. customwas used without further purification in the next step

出典と根拠

ORDレコード
ord-14d096795bba47acbafa6b123602e040
出典データセット
uspto-grants-1981_03
特許番号
US04259336

関連ノート

読み込み中…