HRID5428

反应详情

EQUATION

反应方程式

HRID 5428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-amino-6-chloropyridine (6.43 g, 50 mmoles) and ethyl bromopyruvate (9.75 g, 50 mmoles) in ethanol (150 ml) was heated at reflux for 4 hours. After the solvent was removed, chloroform was added to the residue, which was washed in turn with saturated sodium bicarbonate and saturated saline, and then dried over anhydrous magnesium sulfate. After the solvent was concentrated, n-hexane was added to the mixture. Then, the crystals precipitated were filtered off and washed with n-hexane to obtain 7.60 g of the desired product (67.6%, pale yellow crystals).

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. customAfter the solvent was removed
  3. additionchloroform was added to the residue, which
  4. washwas washed in turn with saturated sodium bicarbonate and saturated saline
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationAfter the solvent was concentrated
  7. additionn-hexane was added to the mixture
  8. customThen, the crystals precipitated
  9. filtrationwere filtered off
  10. washwashed with n-hexane