تفاعل #78266

ord-f15e8082a0c0494ba195fbba2a92a179

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
23°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto reflux under argon for 3.5 hours
  2. 2
    workup.DISTILLATIONthe solvent and excess thionyl chloride were distilled under reduced pressure
  3. 3
    أخرىto remove all traces of thionyl chloride

الإجراء التجريبي

7.4 mL (12.069 g, 101.4 mmol) thionyl chloride and 1.80 g (7.66 mmol) methyl 5-carboxy-1H-benzimidazole-2-carbamate in 37 mL dry benzene were heated to reflux under argon for 3.5 hours. The mixture was then cooled to 23° C. and the solvent and excess thionyl chloride were distilled under reduced pressure. The resulting brown solid was stored under vacuum to remove all traces of thionyl chloride and used in the following Examples without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06710065B1uspto-grants-2004_03