HRID2244399

反应详情

EQUATION

反应方程式

HRID 2244399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A solution of 2-methyl-5-(pyridin-3-ylamino)-thiazole-4-carboxylic acid ethyl ester (0.24 g, 0.90 mmol) in methanol (1.6 ml) was treated with a 2.55 N solution of KOH in water (1.06 ml). The mixture was stirred at 55° C. for 40 min then cooled to room temperature. The volatiles were evaporated and the residue dissolved in water (2.00 ml) and treated with HCl 1N under vigorous stirring until pH 5 was reached. The mixture was stirred for 1 h, then the solids were filtered, washed with water and dried under high vacuum to yield 2-methyl-5-(pyridin-3-ylamino)-thiazole-4-carboxylic acid (0.15 g, 70%) as a light yellow solid, MS (ISP): m/e=234.1 (M−H).

WORKUP

后处理

  1. temperaturethen cooled to room temperature
  2. customThe volatiles were evaporated
  3. dissolutionthe residue dissolved in water (2.00 ml)
  4. additiontreated with HCl 1N
  5. stirringunder vigorous stirring until pH 5
  6. stirringThe mixture was stirred for 1 h
  7. filtrationthe solids were filtered
  8. washwashed with water
  9. customdried under high vacuum