HRID443760

反应详情

EQUATION

反应方程式

HRID 443760 的结构方程式

PROCEDURE

实验过程

Nine grams (0.025 mole) of 3,3'-(6-chloro-s-triazine-2,4-diyl)bis-3-azabicyclo[3.2.2]nonane and 9.7 g. (0.13 mole) n-butylamine is placed in a glass liner in a bomb and then heated in an oil bath maintained at 160°-180° C. for 16 hours. After cooling, the contents of the bomb are rinsed with chloroform and water into a flask and 50 ml. of 10 N NaOH is added. The solution is then evaporated in vacuo and the aqueous solution remaining is extracted with chloroform. The combined chloroform extracts are washed with water, dried over magnesium sulfate, filtered through Magnesol® and the Magnesol® washed with chloroform. Removal of solvent in vacuo, column chromatography on silica gel and recrystallization of the pure fractions containing the major component from n-heptane gives 4.9 g. of colorless prisms, m.p. 101°-103° C.

WORKUP

后处理

  1. temperatureheated in an oil bath
  2. temperaturemaintained at 160°-180° C. for 16 hours
  3. temperatureAfter cooling
  4. washthe contents of the bomb are rinsed with chloroform and water into a flask
  5. additionof 10 N NaOH is added
  6. customThe solution is then evaporated in vacuo
  7. extractionthe aqueous solution remaining is extracted with chloroform
  8. washThe combined chloroform extracts are washed with water
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered through Magnesol®
  11. washthe Magnesol® washed with chloroform
  12. customRemoval of solvent in vacuo, column chromatography
  13. customon silica gel and recrystallization of the pure fractions
  14. additioncontaining the major component from n-heptane
  15. customgives 4.9 g