HRID264331

反应详情

EQUATION

反应方程式

HRID 264331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Methyl 2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methylbutanoate hydrochloride (7164 g, 16.7 mol) is added to a solution of water (27 L) and concentrated hydrochloric acid (9 L), and heated to 120° C. for 3 days. After cooling down to room temperature, charcoal (350 g) is added, stirring is continued for 45 minutes, the reaction is filtered, and the solvent is evaporated. The crude solid is re-dissolved in methanol (7.1 L) and ethyl acetate (73 L), and cooled to 3° C. for 2 hours. The precipitated product is collected by filtration to give 2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methylbutanoic acid hydrochloride.

WORKUP

后处理

  1. temperatureAfter cooling down to room temperature
  2. filtrationthe reaction is filtered
  3. customthe solvent is evaporated
  4. dissolutionThe crude solid is re-dissolved in methanol (7.1 L)
  5. temperatureethyl acetate (73 L), and cooled to 3° C. for 2 hours
  6. filtrationThe precipitated product is collected by filtration