HRID358478

反应详情

EQUATION

反应方程式

HRID 358478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A reaction mixture was prepared from 203 ml. each of triethylamine and pyridine plus 63 g. of morpholinoacetonitrile. Hydrogen sulfide was bubbled through the heated, stirred reaction mixture for about 2.5 hours. Stirring was continued overnight at ambient temperature. The next day, H2S was passed through the heated, stirred reaction mixture for an additional 1.5 hours. At this point, the solvents were evaporated in vacuo and the residue triturated with ether. The ether was discarded and the residue dissolved in ethanol. Crystalline morpholinothioacetamide formed in the above reaction precipitated and was separated by filtration. Treatment of the filtrate with alcoholic hydrogen chloride yielded morpholinothioacetamide hydrochloride melting in the range 64°-80° C. See also J.A.C.S., 72, 2804 (1950).

WORKUP

后处理

  1. customA reaction mixture was prepared from 203 ml
  2. customHydrogen sulfide was bubbled through the heated
  3. customreaction mixture for about 2.5 hours
  4. stirringStirring
  5. stirringstirred
  6. customreaction mixture for an additional 1.5 hours
  7. customAt this point, the solvents were evaporated in vacuo
  8. customthe residue triturated with ether
  9. dissolutionthe residue dissolved in ethanol