HRID1921335

反应详情

EQUATION

反应方程式

HRID 1921335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of the above 2-methoxy-4,6-dimethyl-3-vinylpyridine (0.66 g, 4.05 mmol), 5% palladium on charcoal and ethyl alcohol (10 mL) is stirred under an atmosphere of hydrogen for 4 hr. The catalyst is removed by filtration through a pad of Hi-Flo and the filtrate is concentrated. The residue is purified by chromatography eluting with dichloromethane. Product containing fractions are combined and concentrated to afford 3-ethyl-2-methoxy-4,6-dimethylpyridine (265 mg, 22.4% yield for two steps). LC/MS: MS m/e=166 (M+H); RT 3.76 min; 1H NMR (CDCl3, δ ppm) 6.50 (1H, s), 3.90 (3H, s); 2.58 (2H, q), 2.38 (3H, s); 2.21 (3H, s), 1.07 (3H, t).

WORKUP

后处理

  1. customThe catalyst is removed by filtration through a pad of Hi-Flo
  2. concentrationthe filtrate is concentrated
  3. customThe residue is purified by chromatography
  4. washeluting with dichloromethane
  5. additionProduct containing fractions
  6. concentrationconcentrated