HRID223756

反应详情

EQUATION

反应方程式

HRID 223756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.).

WORKUP

后处理

  1. additionwas added dropwise to the solution over a 3 minute period
  2. temperatureAfter cooling the reaction mixture
  3. customprecipitates
  4. customformed
  5. filtrationwere recovered by filtration
  6. customrecrystallized from a mixture of chloroform and ethanol