تفاعل #310938

ord-92dec17161f442d2b2a367d90b07aabe

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added dropwise to the solution over a 3 minute period
  2. 2
    درجة الحرارةAfter cooling the reaction mixture
  3. 3
    أخرىprecipitates
  4. 4
    أخرىformed
  5. 5
    ترشيحwere recovered by filtration
  6. 6
    أخرىrecrystallized from a mixture of chloroform and ethanol

الإجراء التجريبي

To 30 ml of an ethanol solution of 13.0 g of the intermediate product obtained in Preparative Example 2, viz., 2-ethylmercapto-3-ethylbenzothiazolium p-toluenesulfonate, was added 4.4 g of 3-carboethoxymethylrhodanine, while stirring the mixture at room temperature (about 20° C.), 6.1 g of triethylamine was added dropwise to the solution over a 3 minute period, and thereafter the resultant mixture was refluxed for 10 minutes. After cooling the reaction mixture, precipitates formed were recovered by filtration and recrystallized from a mixture of chloroform and ethanol to provide 1.1 g of 3-carboethoxymethyl-5-(3-ethylbenzothiazolylidene)rhodanine (melting point 250° to 252° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04356247uspto-grants-1982_10