HRID399799

反应详情

EQUATION

反应方程式

HRID 399799 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thionyl chloride (2.5 ml) was added dropwise in methanol (25 ml) under cooling at 7°-9° C. After the mixture was stirred for 30 minutes at the same temperature, 5-(3-methyl-1,2,4-oxadiazol-5-yl)-3-pyridinecarboxylic acid (2.5 g) was added thereto and the mixture was refluxed for 3 hours. After being cooled to room temperature, the mixture was poured into a mixture of ethyl acetate (100 ml) and water (100 ml). The organic layer was successively washed with 10% potassium carbonate aqueous solution and brine, and then dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was recrystallized from diethyl ether to afford methyl 5-(3-methyl-1,2,4-oxadiazol-5-yl)-3-pyridinecarboxylate (2.12 g).

WORKUP

后处理

  1. temperatureunder cooling at 7°-9° C
  2. additionwas added
  3. temperaturethe mixture was refluxed for 3 hours
  4. washThe organic layer was successively washed with 10% potassium carbonate aqueous solution and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated in vacuo
  7. customthe residue was recrystallized from diethyl ether