HRID2393397

反应详情

EQUATION

反应方程式

HRID 2393397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The process is performed as in Example 44 but starting with 3 g of (10 RS)-10-acetamido-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one, 70 ml of dimethyl sulphoxide, 1.2 g of an 80% suspension of sodium hydride in oil and 2.6 ml of 1-bromo-3-phenylpropane. The reaction medium is poured into a mixture of 250 g of ice, 435 ml of distilled water and 6 ml of acetic acid. 200 ml of ethyl acetate are added to the suspension obtained and the mixture is stirred, followed, after separation of the phases once settling has taken place, by removal of the ethyl acetate. The operation is repeated once. The precipitate is filtered off on a sinter funnel. The solid is crystallized from 200 ml of methanol. 390 mg of (10 RS)-10-acetamido-10-(3-phenylpropyl)-5H,10H-imidazo[1,2-a]indeno[1,2-e)pyrazin-4-one are obtained in the form of a green solid melting above 260° C. (Analysis, % calculated C: 72.3, H: 5.6, N: 14.0; % found C: 72.2, H: 5.5, N: 14.2).

WORKUP

后处理

  1. customobtained
  2. customafter separation of the phases
  3. customby removal of the ethyl acetate
  4. filtrationThe precipitate is filtered off on a sinter funnel
  5. customThe solid is crystallized from 200 ml of methanol