HRID1625090

反应详情

EQUATION

反应方程式

HRID 1625090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Sodium hydroxide (74 gm) was added to water (150 ml) at reflux under stirring. Nortropinone hydrochloride (100 gm) was added to the solution and stirred for 20 minutes, and then added benzyl chloride (94 gm) and tetrahydrofuran (300 ml). The contents were heated to reflux and maintained for 15 hours at reflux. The contents were cooled to room temperature and then added hydroxylamine hydrochloride (72 gm) at room temperature. The contents were maintained for 3 hours at room temperature and then added water (200 ml). Sodium hydroxide solution (40%, 50 ml) was added to the reaction mass and then the layers were separated. The aqueous layer was extracted with ethyl acetate and the combined organic layer was dried with sodium sulphate to obtain a crude solid. The crude solid was dissolved in n-hexane (300 ml) and stirred for 1 hour. The separated solid was filtered and dried to obtain 134 gm of 8-benzyl-8-azabicyclo[3.2.1]octan-3-one oxime.

WORKUP

后处理

  1. temperatureat reflux
  2. stirringstirred for 20 minutes
  3. temperatureThe contents were heated
  4. temperatureto reflux
  5. temperaturemaintained for 15 hours
  6. temperatureat reflux
  7. customat room temperature
  8. temperatureThe contents were maintained for 3 hours at room temperature
  9. customthe layers were separated
  10. extractionThe aqueous layer was extracted with ethyl acetate
  11. dry with materialthe combined organic layer was dried with sodium sulphate
  12. customto obtain a crude solid
  13. stirringstirred for 1 hour
  14. filtrationThe separated solid was filtered
  15. customdried