HRID1194552

反应详情

EQUATION

反应方程式

HRID 1194552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A well stirred mixture of 5 g of ethyl 4,6-di-hydroxy-5,6,7,8-tetrahydroquinoline-3-carboxylate and 3.0 g of KHCO3 in 300 mL of CHCl3 is ice-cooled. To the cooled mixture, benzyl chloroformate (3.6 g) is added over a period of 10 minutes maintaining the reaction temperature below 10°. The reaction mixture is vigorously stirred at room temperature overnight, then filtered. The filtrate is washed with H2O, dried (MgSO4), and evaporated to dryness. The dried residue is purified by flash chromatography on a silica gel column to yield ethyl 6-benzyloxycarbonyloxy-4-hydroxy-5,6,7,8-tetrahydroquinoline-3-carboxylate

WORKUP

后处理

  1. temperaturecooled
  2. temperaturemaintaining the reaction temperature below 10°
  3. stirringThe reaction mixture is vigorously stirred at room temperature overnight
  4. filtrationfiltered
  5. washThe filtrate is washed with H2O
  6. dry with materialdried (MgSO4)
  7. customevaporated to dryness
  8. customThe dried residue is purified by flash chromatography on a silica gel column