HRID842702

反应详情

EQUATION

反应方程式

HRID 842702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

6,7-Dichloro-2,3-dimethoxy-5-nitroquinoxaline (20 g, 0.066 mol) and 5% w/w palladium-on-carbon (50% wet) (1.2 g) were suspended in a mixture of tetrahydrofuran (0.12 L) and ethyl acetate (0.12 L). The mixture was hydrogenated at 60° C. and 414 kPa (60 psi) for 22 hours, cooled, diluted with dichloromethane (0.48 L) and the catalyst removed by filtration through celite (trade mark) filter aid. The solution was concentrated under reduced pressure with the gradual addition of toluene. The mixture was then filtered and the solid was washed with toluene (20 ml) to give the title compound as a brown solid (14.2 g, 78%), m.p. 182-4° C.

WORKUP

后处理

  1. customwas hydrogenated at 60° C.
  2. temperaturecooled
  3. customthe catalyst removed by filtration through celite (trade mark)
  4. filtrationfilter aid
  5. concentrationThe solution was concentrated under reduced pressure with the gradual addition of toluene
  6. filtrationThe mixture was then filtered
  7. washthe solid was washed with toluene (20 ml)