HRID1199800

反应详情

EQUATION

反应方程式

HRID 1199800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium t-butoxide (1.01 g) was added to a solution of ethyl amidomalonate (1.38 g) in tetrahydrofuran (38 ml) maintained at 33°. After cooling to 25°, ethyl 4-fluorocinnamate (1.50 g) was added and the mixture stirred overnight at room temperature. Brine was added, the mixture extracted with ethyl acetate (3×60 ml) and the organic solution dried and evaporated to give the crude product. This was chromatographed on silica gel, using dry ether as eluent, to give the title compound (0.92 g, 43%), m.p. 97°-99°.

WORKUP

后处理

  1. temperaturemaintained at 33°
  2. temperatureAfter cooling to 25°
  3. extractionthe mixture extracted with ethyl acetate (3×60 ml)
  4. customthe organic solution dried
  5. customevaporated
  6. customto give the crude product
  7. customThis was chromatographed on silica gel