HRID461667

反应详情

EQUATION

反应方程式

HRID 461667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Acenaphthenequinone, 9.1 g. (0.05m), and 10.3 g. (0.05m) of 4-amino-3-nitrobenzotrifluoride were hydrogenated at room temperature in 125 ml. of 2B ethanol with 2.5 g. of palladium-on-carbon (5 percent) at 50 psi. After 4 hours three equivalents of hydrogen were absorbed and the temperature rose to 40° C. The catalyst was filtered and the filtrate was diluted with 1.2 l. of ethanol. The reaction was completed by refluxing the ethanolic solution for about 1 hour. The precipitated product was collected to yield about 8 g. (50 percent yield) of 9-(trifluoromethyl)acenaphtho[1,2-b]quinoxaline, mp = 185°-186° C.

WORKUP

后处理

  1. customwere hydrogenated at room temperature in 125 ml
  2. customrose to 40° C
  3. filtrationThe catalyst was filtered
  4. additionthe filtrate was diluted with 1.2 l
  5. temperatureby refluxing the ethanolic solution for about 1 hour
  6. customThe precipitated product was collected
  7. customto yield about 8 g