HRID1671676

反应详情

EQUATION

反应方程式

HRID 1671676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 5-(4-fluoro-phenyl)-2-methyl-thiazole-4-carboxylic acid methyl ester (15 g) in a mixture of THF (60 mL) and MeOH (20 mL) was added a solution of sodium hydroxide (2.63 g) in water (60 mL). The reaction mixture was stirred at RT for 30 min. The reaction mixture was then concentrated in vacuo, and the residue was dissolved with water (100 mL) and concentrated again in vacuo. The residue was dissolved in water (250 mL), cooled to 0° C. with a ice-bath. Then was added a solution of conc.HCl (37%)(7.72 g) in water (7.72 g) and stirred at 0° C. for 15 min. The resulting precipitate was filtered off, washed with water and dried in high vacuum pump. to give the title compound as a white solid (13.16 g, 93%).

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated in vacuo
  2. dissolutionthe residue was dissolved with water (100 mL)
  3. concentrationconcentrated again in vacuo
  4. dissolutionThe residue was dissolved in water (250 mL)
  5. temperaturecooled to 0° C. with a ice-bath
  6. additionThen was added a solution of conc
  7. stirringHCl (37%)(7.72 g) in water (7.72 g) and stirred at 0° C. for 15 min
  8. filtrationThe resulting precipitate was filtered off
  9. washwashed with water
  10. customdried in high vacuum pump