HRID904664

反应详情

EQUATION

反应方程式

HRID 904664 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 6-chloro-8-methoxycarbonyl-4-oxo-10-propyl-4H-pyrano[3,2-g]quinoline-2-carboxylate (1.313 g) was suspended in refluxing methanol (300 mls) and 0.1 M sodium hydroxide solution (65 mls) was added dropwise, with stirring. The whole was then refluxed for ten minutes, cooled, poured into water and acidified. The precipitated product was extracted into ethyl acetate, washed with water, dried with magnesium sulphate, filtered and volatiles removed in vacuo, affording 1.05 g of the crude sub-title compound as a yellow solid. This yellow solid was dissolved in sodium bicarbonate solution, filtered and the filtrate acidified. The precipitated product was collected by filtration, washed with water and dried to give 0.77 g of the sub-title compound. MP 340° C.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureThe whole was then refluxed for ten minutes
  3. temperaturecooled
  4. extractionThe precipitated product was extracted into ethyl acetate
  5. washwashed with water
  6. dry with materialdried with magnesium sulphate
  7. filtrationfiltered
  8. customvolatiles removed in vacuo
  9. customaffording 1.05 g of the crude sub-title compound as a yellow solid
  10. filtrationfiltered
  11. filtrationThe precipitated product was collected by filtration
  12. washwashed with water
  13. customdried