HRID535471

反应详情

EQUATION

反应方程式

HRID 535471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

1.69 ml of diethyl ethoxymethylene malonate are added, under an inert atmosphere at ambient temperature, to 1.83 g (6.8 mmol) of (4-aminophenyl)(2-methylindolizin-3-yl)methanone in 23 ml of toluene. The reaction medium is heated at 110° C. for 1 h 45 and then concentrated under reduced pressure. The residue obtained is dissolved in 45 ml of diphenyl ether and then heated at 230° C. for 30 minutes. After the addition of diisopropyl ether at ambient temperature, the precipitate formed is filtered off, rinsed with diisopropyl ether, with methanol and then with dichloromethane, and dried under reduced pressure at 50° C. overnight 1.2 g of a yellow powder are obtained.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customThe residue obtained
  3. temperatureheated at 230° C. for 30 minutes
  4. customthe precipitate formed
  5. filtrationis filtered off
  6. washrinsed with diisopropyl ether, with methanol
  7. dry with materialwith dichloromethane, and dried under reduced pressure at 50° C. overnight 1.2 g of a yellow powder
  8. customare obtained