HRID1818889

反应详情

EQUATION

反应方程式

HRID 1818889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-chloro-4,6-dimethyl-nicotinonitrile (2.5 g, 15.01 mmol) was dissolved in anhydrous methanol(70 mL), added with sodium methoxide (4.27 g, 75.03 mmol) at 0° C. and stirred for about 10 hours at nitrogen atmosphere. The above mixture was concentrated under reduced pressure and then neutrailized with a saturated solution of ammonium chloride and then extracted twice with 150 mL of methylenechloride. The resulting organic layer was dried using anhydrous sodium sulfate, filtered and concentrated. A silica gel column chromatography (20% EtOAc/Hexanes) was performed on the resulting residue and 2.41 g (99%) of 2-methoxy-4,6-dimethyl-nicotinonitrile was obtained in white solid.

WORKUP

后处理

  1. concentrationThe above mixture was concentrated under reduced pressure
  2. extractionextracted twice with 150 mL of methylenechloride
  3. customThe resulting organic layer was dried
  4. filtrationfiltered
  5. concentrationconcentrated