HRID277376

反应详情

EQUATION

反应方程式

HRID 277376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A sodium ethoxide solution (previously prepared from ethanol and sodium (1.00 g, 0.0430 mol)) is cooled with an ice-acetone bath, treated portionwise with ethyl cyanoacetate (4.51 g, 0.0398 mol), stirred at room temperature for 30 minutes, treated with 3-chloro-5-nitro-1,2-benzisothiazole (4.27 g, 0.0199 mol), stirred at room temperature overnight, cooled to 0° C., and treated dropwise with 10% hydrochloric acid (15.0 mL). The resultant aqueous mixture is stirred at room temperature for one hour and filtered to obtain a solid. The solid is washed with ethanol and air-dried to give the title product as a yellow solid which is identified by NMR spectral analysis.

WORKUP

后处理

  1. temperatureis cooled with an ice-acetone bath
  2. stirringstirred at room temperature overnight
  3. temperaturecooled to 0° C.
  4. stirringThe resultant aqueous mixture is stirred at room temperature for one hour
  5. filtrationfiltered
  6. customto obtain a solid
  7. washThe solid is washed with ethanol
  8. customair-dried