تفاعل #11347

ord-65102f31262e4021b5784cb373f3c5c1

معادلة التفاعل

O=S(Cl)Cl
Thionyl chloride
O=S(=O)(O)c1ccc2ncsc2c1
benzothiazole-6-sulfonic acid
CN(C)C=O
dimethylformamide
O=S(=O)(Cl)c1ccc2ncsc2c1
6-Chlorosulfonylbenzothiazole

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction mixture was heated
  2. 2
    درجة الحرارةat reflux
  3. 3
    أخرىto yield a clear solution
  4. 4
    درجة الحرارةat reflux
  5. 5
    أخرىthe solvent was removed in vacuo and excess HCl and thionyl chloride
  6. 6
    أخرىwas chased by evaporation with dichloroethane

الإجراء التجريبي

Thionyl chloride (4 mL) was added to a suspension of the benzothiazole-6-sulfonic acid (0.60 g, 2.79 mmol) in dichloroethane (15 mL) and the reaction mixture was heated at reflux and dimethylformamide (5 mL) was added to the reaction mixture to yield a clear solution. After 1.5 hr. at reflux, the solvent was removed in vacuo and excess HCl and thionyl chloride was chased by evaporation with dichloroethane.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07098202B2uspto-grants-2006_08