HRID1964790

反应详情

EQUATION

反应方程式

HRID 1964790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-tosyloxy-6-acetoxymethylpyridine (50 g, 0.148 mol) and NaOH (25 g, 0.62 mol) in 150 mL of water was refluxed for 15 h. The reaction mixture was cooled to RT and neutralized with con. HCl. The solvent was evaporated under vacuum affording a solid residue, which was suspended in ethyl acetate (750 mL) and heated to 60° C. for 30 min. with stirring. The suspended material was filtered off and the filtrate was concentrated to give 5-hydroxy-2-hydroxymethylpyridine (15 g, 80%) as a pale yellow solid. It was used in next step without further purification.

WORKUP

后处理

  1. temperaturewas refluxed for 15 h
  2. customThe solvent was evaporated under vacuum
  3. customaffording a solid residue, which
  4. temperatureheated to 60° C. for 30 min.
  5. filtrationThe suspended material was filtered off
  6. concentrationthe filtrate was concentrated