HRID1685

反应详情

EQUATION

反应方程式

HRID 1685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 2-ethyl nicotinic acid lithium salt (5 g, 3.18 mmol) in distilled THF (400 mL) under nitrogen was cooled to 0° C. and lithium aluminum hydride (1M in THF) (25 mL) was added dropwise. The reaction was stirred for 3 hours at room temperature then cooled to 0° C. and quenched with EtOAc (949 μL), then H2O (949 μL), then 15% NaOH (949 μL), followed by H2O (2.8 mL). The solution was filtered and the solvent removed under reduced pressure. Toluene was added and the solvent was removed under reduced pressure to give the desired 2-ethyl-3 -hydroxymethylpyridine.

WORKUP

后处理

  1. temperaturethen cooled to 0° C.
  2. customquenched with EtOAc (949 μL)
  3. filtrationThe solution was filtered
  4. customthe solvent removed under reduced pressure
  5. additionToluene was added
  6. customthe solvent was removed under reduced pressure