HRID23939

反应详情

EQUATION

反应方程式

HRID 23939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Morpholine (1.9 ml; 21.8 mmol) was added to a solution of 5-chloromethyl-8-hydroxyquinoline (1.98 g; 8.34 mmol) in CHCl3 (50 ml) at 5° C. The reaction mixture was stirred overnight at room temperature. Then CHCl3 (100 ml) was added and the solution was washed with 5% NaHCO3 (2×50 ml), followed by brine (50 ml), and dried over Na2SO4. The solution was filtered and evaporated under vacuum to dryness. The residue was crystallized from hexane-CHCl3 and gave 1.2 g (59%) of the title product. M.p. 130° C. TLC (CHCl3; MeOH; NH3=8:2:0.5. Rf=0.69.

WORKUP

后处理

  1. washthe solution was washed with 5% NaHCO3 (2×50 ml)
  2. dry with materialdried over Na2SO4
  3. filtrationThe solution was filtered
  4. customevaporated under vacuum to dryness
  5. customThe residue was crystallized from hexane-CHCl3