HRID544447

反应详情

EQUATION

反应方程式

HRID 544447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.86 g. of 3-chloro-4-oxopentanonitrile, 0.92 g. of 2-amino-3-phenylmethoxypyridine and 0.5 ml. of triethylamine in 15 ml. of ethanol was stirred for 16 hours, then concentrated to remove the triethylamine and ethanol. The residue was dissolved in methylene chlorideand washed with water. The methylene chloride was concentrated and the residual oil was dissolved in 20 ml. of boiling acetonitrile, filtered, cooled, and treated with hydrogen chloride/methanol with cooling to give 0.22 g. of the desired product (m.p. 163°-166° C.).

WORKUP

后处理

  1. concentrationconcentrated
  2. customto remove the triethylamine and ethanol
  3. dissolutionThe residue was dissolved in methylene
  4. washchlorideand washed with water
  5. concentrationThe methylene chloride was concentrated
  6. dissolutionthe residual oil was dissolved in 20 ml
  7. filtrationof boiling acetonitrile, filtered
  8. temperaturecooled
  9. additiontreated with hydrogen chloride/methanol
  10. temperaturewith cooling
  11. customto give 0.22 g