HRID55870

反应详情

EQUATION

反应方程式

HRID 55870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

5-Nitro-2-chloropyridine (21) (350 mg, 2.21 mmol) and 1-Boc-piperazine (430 mg, 2.31 mmol) were dissolved in MeCN (3.6 mL). TEA (400 μL, 2.87 mmol) was added and the mixture heated at 140° C. in the microwave (250 W, stirring) for 30 minutes. The solvent was evaporated in vacuo and the residue dissolved in DCM (75 mL). The solution was washed with 0.5N HCl (2×20 mL) and the organic phase washed with saturated brine solution (40 mL), then dried (MgSO4), filtered and the solvent evaporated in vacuo to afford the title compound as a yellow solid (646 mg, 95%); LCMS, Rt=2.97 min (MeOH-FA method), m/z 309 (MH+).

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. dissolutionthe residue dissolved in DCM (75 mL)
  3. washThe solution was washed with 0.5N HCl (2×20 mL)
  4. washthe organic phase washed with saturated brine solution (40 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent evaporated in vacuo