HRID399801

反应详情

EQUATION

反应方程式

HRID 399801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of methyl 5-tert-butoxycarbonylamino-3-pyridinecarboxylate (5.7 g) and conc. hydrochloric acid (11.4 ml) in methanol (57 ml) was stirred for 1 hour at 40° C. After being cooled to room temperature, the reaction mixture was poured into a mixture of ethyl acetate (100 ml) and water (50 ml) under stirring, and adjusted to pH 9.0 with 10% potassium carbonate aqueous solution. The organic layer was washed with brine and dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was recrystallized from diethyl ether-methanol to afford methyl 5-amino-3-pyridinecarboxylate (2.03 g).

WORKUP

后处理

  1. temperatureAfter being cooled to room temperature
  2. stirringunder stirring
  3. washThe organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated in vacuo
  6. customthe residue was recrystallized from diethyl ether-methanol