HRID7163

反应详情

EQUATION

反应方程式

HRID 7163 的结构方程式

PROCEDURE

实验过程

A solution of 2-pyrazinecarboxylic acid (2.00 g, 16.1 mmol) and H2SO4 (catalytic) in MeOH (50 mL) was heated at reflux for 45 minutes, then concentrated in vacuo. The residue was partitioned between EtOAc (40 mL) and saturated NaHCO3(aq) (20 mL). The organic phase was washed with saturated NaHCO3(aq) (20 mL) and brine (10 mL), then dried (MgSO4) and concentrated in vacuo to give colourless crystals (1.32 g, 59%). 1H NMR (CDCl3) □ 4.04 (s, 3H), 8.72 (dd, 11H, J=2.4, 1.2 Hz), 8.77 (d, 1H, J=2.4 Hz), 9.32 (d, 1H, J=1.2 Hz).

WORKUP

后处理

  1. temperatureat reflux for 45 minutes
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between EtOAc (40 mL) and saturated NaHCO3(aq) (20 mL)
  4. washThe organic phase was washed with saturated NaHCO3(aq) (20 mL) and brine (10 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo