HRID65927

反应详情

EQUATION

反应方程式

HRID 65927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl bromopyruvate (8.0 g, 0.1041 m) and ethyl 4-quinazolylacetate prepared according to the procedure of Elderfield and Serlin, J. Org. Chem. 16, 1669 (1951) (2.32 g, 0.011 m) in dry EtOH (250 ml) was heated at reflux for 24 hr. Sodium bicarbonate was added until effervescence ceased. A solid formed and this was filtered, washed well with H2O, and dried. The crude product (1.8 g) was chromatographed on 150 g of Silicar. The desired product was eluted with 3% EtOAc/benzene. Crystallization from MeOH afforded the desired product as a white solid; m.p. 125°-126° C.

WORKUP

后处理

  1. temperatureat reflux for 24 hr
  2. customA solid formed
  3. filtrationthis was filtered
  4. washwashed well with H2O
  5. customdried
  6. customThe crude product (1.8 g) was chromatographed on 150 g of Silicar
  7. washThe desired product was eluted with 3% EtOAc/benzene
  8. customCrystallization from MeOH