HRID864755

反应详情

EQUATION

反应方程式

HRID 864755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of isonicotinic acid (0.98 g, 0.008 mol), 2-bromomethylsaccharin (2.11 g, 0.008 mol), triethylamine (0.81 g, 0.008 mol) and xylene (25 ml) were refluxed for 1 hour. The solvent was removed in vacuo and the residue was partitioned between water and methylene chloride. The organic layer was separated and the solvent removed in vacuo. The solid residue was recrystallized from CH3CN to afford 0.9 g (37%) of 2-saccharinylmethyl pyridine-4-carboxylate as a yellow solid, m.p. 145°-146° C.

WORKUP

后处理

  1. temperaturewere refluxed for 1 hour
  2. customThe solvent was removed in vacuo
  3. customthe residue was partitioned between water and methylene chloride
  4. customThe organic layer was separated
  5. customthe solvent removed in vacuo
  6. customThe solid residue was recrystallized from CH3CN