HRID1278466

反应详情

EQUATION

反应方程式

HRID 1278466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 19.42 g. portion of 2-(2-pyridyl)-2-phenylacetonitrile was stirred with 4.8 g. of 50% sodium hydride in 50 ml. of dimethylformamide, and reacted with 7.65 g. of 4-chloromethylimidazole hydrochloride in 25 ml. of dimethylformamide as described in Example 1. The mixture was stirred at 80°-90° C. for 1 hour, the solvent was removed by evaporation under vacuum, and wthe residue was worked up as described in Example 1 to obtain 11.87 g. of the free base named in the heading above, m.p. 111°-115° C. dec. The product was triturated twice with portions of diethyl ether, and was dissolved in chloroform. The solution was extracted with water and dried over sodium sulfate. Evaporation of the solvent under vacuum gave 11.84 g. of purified free base, m.p. 111°-115° C.

WORKUP

后处理

  1. customthe solvent was removed by evaporation under vacuum
  2. customto obtain 11.87 g
  3. customThe product was triturated twice with portions of diethyl ether
  4. dissolutionwas dissolved in chloroform
  5. extractionThe solution was extracted with water
  6. dry with materialdried over sodium sulfate
  7. customEvaporation of the solvent under vacuum
  8. customgave 11.84 g