HRID1701400

反应详情

EQUATION

反应方程式

HRID 1701400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-amino-3-ethylpyridine (13.0 g., 0.1063 mole) and ethyl ethoxymethylenecyanoacetate (18.0 g., 0.1063 mole) in toluene (50 ml.) was heated on a steam bath for 20 minutes. The solution was cooled and the resulting mixture diluted with Skellysolve B. The title compound (19.0 g.), m.p. 122°-125° C., was collected by filtration. From the mother liquors, after recrystallization from cyclohexane, was obtained a further crop (7.0 g.) of product, m.p. 122°-125° C. Total yield of title compound, 26.0 g. (99.6%). The material from cyclohexane was recrystallized twice from methanol to give analytical material, m.p. 123°-125° C.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. filtrationThe title compound (19.0 g.), m.p. 122°-125° C., was collected by filtration
  3. customFrom the mother liquors, after recrystallization from cyclohexane
  4. customwas obtained a further crop (7.0 g.) of product, m.p. 122°-125° C