HRID65779

反应详情

EQUATION

反应方程式

HRID 65779 的结构方程式

PROCEDURE

实验过程

6.2 g. of 4-chloro-1-ethyl-5,6-dihydrobenzo[5,6]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridin-11(1H)-one (0.02 mol.) are added to a solution of 0.5 g. of sodium (0.022 mol.) in 150 ml. of absolute ethanol. The mixture is heated at 120° (bath temperature) in an autoclave for 4 hours. After cooling, the crystallized 4-ethoxy-1-ethyl-5,6-dihydrobenzo[5,6]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridin-11(1H)-one is filtered off and washed with water; yield: 3.5 g. An additional crop of 2.1 g. is obtained by work up of the mother liquor, total yield: 5.6 g. (87.5%). m.p. 150°-152° (recrystallized from ethanol).

WORKUP

后处理

  1. temperatureThe mixture is heated at 120° (bath temperature) in an autoclave for 4 hours
  2. temperatureAfter cooling
  3. filtrationthe crystallized 4-ethoxy-1-ethyl-5,6-dihydrobenzo[5,6]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridin-11(1H)-one is filtered off
  4. washwashed with water
  5. customis obtained by work up of the mother liquor, total yield: 5.6 g
  6. customm.p. 150°-152° (recrystallized from ethanol)