HRID2106799

反应详情

EQUATION

反应方程式

HRID 2106799 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Two ml of 48 percent hydrobromic acid were added with stirring to mixture of 1.38 g (5.5 mol) of 2-methoxy-3-methyl-5-(trifluoromethyl)pyridine and 6 ml of glacial acetic acid at 100° C. and the mixture was allowed to react at about 95° C. for 20 min. The mixture was then cooled and poured onto ice and the solid that formed was collected by filtration. A second crop of solid was obtained by adding more water to the filtrate. The combined solids were dried to obtain 0.40 g (40 percent of theory) of the title compound as a white powder melting at 141°-143° C. The proton nmr spectrum was consistent with the assigned structure.

WORKUP

后处理

  1. customto react at about 95° C. for 20 min
  2. temperatureThe mixture was then cooled
  3. additionpoured onto ice
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. customA second crop of solid was obtained
  7. customThe combined solids were dried