HRID2264352

反应详情

EQUATION

反应方程式

HRID 2264352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Stir 3-bromo-2-methyl-6-nitro-pyridine (2.46 g), 1-isopropyl-piperazine (2.74 g), tetra-n-butyl ammonium iodide (418.69 mg) and potassium carbonate (1.72 g) in dimethyl sulfoxide (DMSO, 20 mL) at 65° C. overnight. Add EA and water, separate the phases and dry the organic layer over magnesium sulfate and remove the solvent under vacuum. Purify by strong cation exchange cartridge eluting with methanol and then methanol-NH3 2 N to afford 2.58 g of the title compound. MS (ES+): m/z=265 (M+H)+

WORKUP

后处理

  1. customAdd EA and water, separate the phases
  2. dry with materialdry the organic layer over magnesium sulfate
  3. customremove the solvent under vacuum
  4. customPurify by strong cation exchange cartridge
  5. washeluting with methanol