HRID544447
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationconcentrated
- customto remove the triethylamine and ethanol
- dissolutionThe residue was dissolved in methylene
- washchlorideand washed with water
- concentrationThe methylene chloride was concentrated
- dissolutionthe residual oil was dissolved in 20 ml
- filtrationof boiling acetonitrile, filtered
- temperaturecooled
- additiontreated with hydrogen chloride/methanol
- temperaturewith cooling
- customto give 0.22 g