HRID535456

反应详情

EQUATION

反应方程式

HRID 535456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.92 ml (4.92 mmol) of a 1N aqueous solution of sodium hydroxide are added, at ambient temperature, to 1.91 g (4.69 mmol) of methyl 2-amino-5-[(1-bromo-2-methylindolizin-3-yl)carbonyl]benzoate in 30 ml of methanol. The reaction medium is refluxed for 10 hours and then hydrolysed with a 1N aqueous solution of hydrochloric acid. The aqueous phase is extracted with ethyl acetate. The organic phase obtained is washed with water, dried over sodium sulphate, filtered, and concentrated under reduced pressure. The solid obtained is rinsed with diisopropyl ether and dichloromethane, and dried under reduced pressure overnight at 50° C. 1.55 g of a yellow solid are obtained.

WORKUP

后处理

  1. temperatureThe reaction medium is refluxed for 10 hours
  2. extractionThe aqueous phase is extracted with ethyl acetate
  3. customThe organic phase obtained
  4. washis washed with water
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe solid obtained
  9. washis rinsed with diisopropyl ether and dichloromethane
  10. customdried under reduced pressure overnight at 50° C