HRID54621

反应详情

EQUATION

反应方程式

HRID 54621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl bromoacetate (24 ml; 0.15 mol) is slowly added dropwise, at room temperature, to a suspension of N4 -benzoylcytosine (21.5 g; 0.1 mol) and potassium carbonate 13.8 g; 0.1 mol) in anhydrous N,N-dimethylformamide (2.15 l). The heterogeneous mixture is stirred vigorously at room temperature for 20 h and insoluble starting material is subsequently filtered off with suction; the filtrate is concentrated in vacuo and the residue is subsequently distilled repeatedly with toluene and then taken up in chloroform (1.0 l); it is then extracted once by shaking with water (0.3 l), and the phases are swiftly separated. The organic phase is filtered once more and concentrated. Yield: 15.23.g (46%).

WORKUP

后处理

  1. filtrationis subsequently filtered off with suction
  2. concentrationthe filtrate is concentrated in vacuo
  3. distillationthe residue is subsequently distilled repeatedly with toluene
  4. extractionit is then extracted once
  5. stirringby shaking with water (0.3 l)
  6. customthe phases are swiftly separated
  7. filtrationThe organic phase is filtered once more
  8. concentrationconcentrated