HRID2173364

反应详情

EQUATION

反应方程式

HRID 2173364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a mixture of ethyl 2-(6-amino-2-methylpyridin-3-yl)propanoate (1.6 g, 7.6 mmol), CH(OEt)3 (3.4 g, 22.8 mmol) in AcOH (50 mL) was added NaN3 (0.6 g, 9.2 mmol) at room temperature. The mixture was heated to 90° C. and stirred for 50 min. The mixture was cooled to ambient temperature and stand over night. The mixture was concentrated under reduce pressure. Water was added, and the mixture was extracted with EtOAc. The combined organic layer was washed with brine, dried over anhydrous Na2SO4, concentrated and the residue was purified by column chromatograph to give compound ethyl 2-[2-methyl-6-(1H-tetrazol-1-yl)pyridin-3-yl]propanoate.

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. waitstand over night
  3. concentrationThe mixture was concentrated
  4. additionWater was added
  5. extractionthe mixture was extracted with EtOAc
  6. washThe combined organic layer was washed with brine
  7. dry with materialdried over anhydrous Na2SO4
  8. concentrationconcentrated
  9. customthe residue was purified by column chromatograph