HRID2380242

反应详情

EQUATION

反应方程式

HRID 2380242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5,11-Dihydro-11-ethyl-5-methyl-2-trifluoromethanesulfonyloxy-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.25 g) was dissolved in pyrrolidine (1 ml) and refluxed 30 min. The cooled solution was diluted with ethyl acetate, washed with water, and the organic phase was dried (anhydrous magnesium sulfate) and concentrated. The resulting oily residue was crystallized from ethyl acetate/hexane to provide 0.11 g of 5,11-dihydro-11-ethyl-5-methyl-2-n-(pyrrolidino-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, m.p. 185°-188° C.

WORKUP

后处理

  1. temperaturerefluxed 30 min
  2. washwashed with water
  3. dry with materialthe organic phase was dried (anhydrous magnesium sulfate)
  4. concentrationconcentrated
  5. customThe resulting oily residue was crystallized from ethyl acetate/hexane