HRID224588

反应详情

EQUATION

反应方程式

HRID 224588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 4 g of the ester of Example 1, 2.45 ml of dimethylaminoethanol and 50 ml of anhydrous toluene was heated to reflux and then cooled to 50° C. and 95 mg of a 50% sodium hydride oil suspension was added thereto. The mixture was again heated to reflux and was then cooled to 40° C. and 0.2 ml of acetic acid were added thereto. The mixture was evaporated to dryness and the residue was dissolved in methylene chloride. The solution was filtered and the filtrate was washed with water, dried and filtered. The filtrate was evaporated to dryness to obtain 4.01 g of 2-dimethylaminoethyl 2-(7-chloro-4-quinolinylamino)-5-fluorobenzoate.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperatureThe mixture was again heated
  4. temperatureto reflux
  5. temperaturewas then cooled to 40° C.
  6. customThe mixture was evaporated to dryness
  7. dissolutionthe residue was dissolved in methylene chloride
  8. filtrationThe solution was filtered
  9. washthe filtrate was washed with water
  10. customdried
  11. filtrationfiltered
  12. customThe filtrate was evaporated to dryness