HRID1640459

反应详情

EQUATION

反应方程式

HRID 1640459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(4-Chlorobutyl)-5-methyl-1H-pyrimidine-2,4-dione (0.69 mmol, 0.15 g), 1-(2,4-dichlorobenzyl)piperazine (0.62 mmol, 0.15 g), sodium bromide (3.46 mmol, 0.36 g) and diisopropylethylamine (6.92 mmol, 0.89 g) were heated in N-methylpyrrolidinone (0.6 ml) at 120° C. for 5 hours. The reaction mixture was then allowed to cool, the suspension was filtered with suction, and the filtrate was concentrated. The residue was then then taken up in ethyl acetate and washed with saturated brine. The organic layer was dried, filtered to remove the desiccant and evaporated in vacuo. The resulting residue was purified by chromatography on silica gel (eluent: methyl tert-butyl ether/methanol (0-100%), resulting in 88.0 mg of the title compound.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationthe suspension was filtered with suction
  3. concentrationthe filtrate was concentrated
  4. washwashed with saturated brine
  5. customThe organic layer was dried
  6. filtrationfiltered
  7. customto remove the desiccant and
  8. customevaporated in vacuo
  9. customThe resulting residue was purified by chromatography on silica gel (eluent