HRID1414516

反应详情

EQUATION

反应方程式

HRID 1414516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2 g of sodium amide are added to a suspension of 9.5 g of 1-methyl 1,2,4,5-tetrahydro 2,4-diketo 3-H-1,5-benzodiazepine, obtained in the example XIV, in 30 c.c. of xylene, and the whole is heated for about thirty minutes, while agitating, treated with 20 c.c. of methyl-sulfate and as soon as the exothermic reaction has ceased, this is heated and boiled for three hours. The solvent is evaporated under reduced pressure, the residue is taken up in 200 c.c. of a 10% solution of caustic soda, and after agitation, suction filtered, and purified upon crystallisation in 90% ethanol. Yield 4.5 g; melting point : 240°-242° C. Analysis: C11H12N2O2Calculated: C % 64.69 H % 5.92; N % 13.72; Found: 64.67; 6.12; 13.95.

WORKUP

后处理

  1. customobtained in the example XIV, in 30 c.c
  2. additiontreated with 20 c.c
  3. temperaturethis is heated
  4. customThe solvent is evaporated under reduced pressure
  5. filtrationof a 10% solution of caustic soda, and after agitation, suction filtered
  6. custompurified upon crystallisation in 90% ethanol
  7. custom240°-242° C