HRID258538

反应详情

EQUATION

反应方程式

HRID 258538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3.03 g of 7-chloro-5-phenyl-1H-1,5-benzodiazepin-4-one-2-thione in a solution of 0.40 g of sodium hydroxide and 15 ml of methanol is added, with stirring a solution of 1.4 g of methyl iodide in 10 ml of methanol. Stirring is continued for 1 hour, the reaction is then evaporated and suspended in methylene chloride (30 ml). The suspension is filtered through a short Florisil column; the column is washed with ethyl acetate and the combined filtrates are evaporated. The residue is triturated with a minimum amount of absolute ethanol and the title compound is filtered off and dried.

WORKUP

后处理

  1. customthe reaction is then evaporated
  2. filtrationThe suspension is filtered through a short Florisil column
  3. washthe column is washed with ethyl acetate
  4. customthe combined filtrates are evaporated
  5. customThe residue is triturated with a minimum amount of absolute ethanol
  6. filtrationthe title compound is filtered off
  7. customdried