HRID1696917

反应详情

EQUATION

反应方程式

HRID 1696917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,6-dichloro-4-methyl-nicotinamide (6.40 g) in 2:1 acetic anhydride/acetic acid (156 mL) was treated with sodium nitrite (21.5 g), stirred for 18 hours, poured into diethyl ether (600 mL) and filtered. The filtrate was concentrated with a toluene azeotrope, and the concentrate was treated with brine and extracted with ethyl acetate. The extract was dried (MgSO4), filtered, and concentrated; and this concentrate was suspended in hexane, sonicated and filtered.

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated with a toluene azeotrope
  3. additionthe concentrate was treated with brine
  4. extractionextracted with ethyl acetate
  5. dry with materialThe extract was dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customsonicated
  9. filtrationfiltered