HRID358556

反应详情

EQUATION

反应方程式

HRID 358556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2 g (8.4 mmol) of 4-pyridylcarbamoyl-beta-alanine ethyl ester and 0.37 g (9.2 mmol) of sodium hydroxide in 50 ml of methanol and 0.1 ml of water is kept agitated for 24 hr at room temperature. After concentration to dryness, the resulting oily residue is taken up in 15 ml of water. After washing with 3 x 10 ml of dichloromethane, the aqueous phase is acidified with a 3 N hydrochloric acid solution until a pH close to 3 is obtained. The precipitate formed is filtered, washed with 10 ml of cold water and then dried 1.36 g (yield 95%) of 4-pyridylcarbamoyl-beta-alanine is obtained in the form of a solid having a melting point of 222° C.

WORKUP

后处理

  1. concentrationAfter concentration to dryness
  2. washAfter washing with 3 x 10 ml of dichloromethane
  3. customa pH close to 3
  4. customis obtained
  5. customThe precipitate formed
  6. filtrationis filtered
  7. washwashed with 10 ml of cold water