HRID1070517

反应详情

EQUATION

反应方程式

HRID 1070517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethyl glycolate (1.04 g) was dissolved in tetrahydrofuran (10 ml) and the solution was cooled to 0° C. Sodium hydride (60% suspension in oil, 0.43 g) was added and the suspension was stirred and then sonicated in an ultrasonic bath. 2-Chloropyrimidine (1.14 g) was added and the mixture was sonicated for a further 110 min. Ammonium chloride solution was added and the mixture was extracted thrice with ethyl acetate, the organic phases were washed with brine and dried, filtered and evaporated. The residue was purified by chromatography eluting with iso-hexane:ethyl acetate (13:7) to give the subtitle compound (1.40 g) as an oil.

WORKUP

后处理

  1. customsonicated in an ultrasonic bath
  2. customthe mixture was sonicated for a further 110 min
  3. extractionthe mixture was extracted thrice with ethyl acetate
  4. washthe organic phases were washed with brine
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was purified by chromatography
  9. washeluting with iso-hexane:ethyl acetate (13:7)