HRID636570

反应详情

EQUATION

反应方程式

HRID 636570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 cm3 of 5N sodium hydroxide is added with stirring to a solution of 0.34 g of methyl 2-bromo-3-(3-pyridyl)-5,6,7,8-tetrahydroindolizine-1-carboxylate in methanol at 20° C. The orangy solution is heated to reflux for 15 hours. The solvent is then evaporated off at reduced pressure (2.7 kPa) at a temperature close to 40° C. The residue is taken up with 10 cm3 of water and acidified to pH˜3 with 0.2 cm3 of 12N hydrochloric acid and 0.5 cm3 of 1N acetic acid. The precipitate is filtered off, washed with water and then dried in air. 0.29 g of 2-bromo-3-(3-pyridyl)-5,6,7,8-tetrahydroindolizine-1-carboxylic acid are thus obtained in the form of a cream powder which melts at >260° C., with decomposition.

WORKUP

后处理

  1. temperatureThe orangy solution is heated
  2. temperatureto reflux for 15 hours
  3. customThe solvent is then evaporated off at reduced pressure (2.7 kPa) at a temperature
  4. customclose to 40° C
  5. filtrationThe precipitate is filtered off
  6. washwashed with water
  7. customdried in air