HRID7151

反应详情

EQUATION

反应方程式

HRID 7151 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-ethoxypicolinic acid (0.202 g, 1.21 mmol) in dry THF (1 mL) was added BH3.THF (1.0 M in THF, 5.0 mL, 5.0 mmol) and the reaction mixture stirred at room temperature for 2.5 hours. The mixture was then quenched with methanol (20 mL), stirred at reflux for 4 hours and concentrated under reduced pressure. The resultant crude product was dissolved in methanol (3×15 mL) and concentrated to give the desired crude alcohol (0.231 g) as an orange solid. 1H NMR (CDCl3): δ 1.46 (t, 3H, J=7.0 Hz), 4.07 (q, 2H, J=7.0 Hz), 4.74 (s, 2H), 7.09–7.20 (m, 2H), 8.14 (d, 1H, J=4.5 Hz).

WORKUP

后处理

  1. customThe mixture was then quenched with methanol (20 mL)
  2. stirringstirred
  3. temperatureat reflux for 4 hours
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe resultant crude product was dissolved in methanol (3×15 mL)
  6. concentrationconcentrated