HRID7163
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureat reflux for 45 minutes
- concentrationconcentrated in vacuo
- customThe residue was partitioned between EtOAc (40 mL) and saturated NaHCO3(aq) (20 mL)
- washThe organic phase was washed with saturated NaHCO3(aq) (20 mL) and brine (10 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo