HRID423216

反应详情

EQUATION

反应方程式

HRID 423216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
62.5 °C

PROCEDURE

实验过程

Ethyl (S)-2-ethoxy-4-[N-(1-(2-piperidino-phenyl)-3-methyl-1-butyl)-amino carbonylmethyl]-benzoate (4.5 g, 0.0093 mol) was dissolved in methanol (45 ml), followed by the addition of sodium hydroxide solution (0.75 g of sodium hydroxide dissolved in 6 ml water). The reaction mixture was heated at 60-65° C. for 3-4 hours. Methanol (80-85%) was removed from the reaction mixture under vacuum. The remaining reaction mixture was diluted with water (45 ml) and pH was adjusted to 6.5-7.0 with 1N HCl. The precipitated solid was stirred for 2-3 hours followed by filtration and washing with water (45 ml). The product was further dried at 50-55° C. under vacuum for 6-8 hours to produce Repaglinide (Yield=83.2%; HPLC Purity: 99.89%).

WORKUP

后处理

  1. customMethanol (80-85%) was removed from the reaction mixture under vacuum
  2. customThe remaining reaction mixture
  3. filtrationfollowed by filtration
  4. washwashing with water (45 ml)
  5. customThe product was further dried at 50-55° C. under vacuum for 6-8 hours