Hydrochloric Acid → HCID 53652618, 화합물

HRID 128256

반응식

HRID 128256 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 53652618HCID 53652618, 화합물

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-14d096795bba47acbafa6b123602e040
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259336

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