تفاعل #926744

ord-c553a41648a14f748b5d6a279185da3f

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىobtained
  2. 2
    درجة الحرارةThe reaction is maintained at 0° to 5° C. for 48 hr
  3. 3
    أخرىand the solvent and excess hydrogen chloride removed under reduced pressure
  4. 4
    أخرىof dry benzene and collected
  5. 5
    أخرىprovides 13.0 g

الإجراء التجريبي

Hydrogen chloride is bubbled through a mixture of 4-cyanostilbene (13.5 g., 0.065 mole), obtained according to the method of Belgian Pat. No. 641,415 (Chem. Abs. 63: 3092g (1965)), in 35 ml. of dry benzene and 17.5 ml. of absolute ethanol at 0° to 5° C. for a period of 3 hr. The reaction is maintained at 0° to 5° C. for 48 hr. and the solvent and excess hydrogen chloride removed under reduced pressure. The residue stirred with 50 ml. of dry benzene and collected provides 13.0 g. of ethyl-4-styrylbenzimidate hydrochloride. A methanol solution of the benzimidate salt is cooled to 5° to 10° C., saturated with ammonia and heated at a temperature of 100° C. for a period of 3 hr. in an enclosed container. Concentration of the reaction mixture provides 4-styrylbenzamidine hydrochloride.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04096183uspto-grants-1978_06