HRID1591153

反应详情

EQUATION

反应方程式

HRID 1591153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3.66 g (12.0 mmoles) 1'-benzoyl-1,3-dihydro-1-oxospiro-[2H-indene-2,4'-piperidine] in 90 ml ethanol and 30 ml 6N hydrochloric acid was heated at reflux for 42 hours. An additional 10 ml 6N hydrochloric acid was added and the solution was heated at reflux for 6 hours. The cooled solution was concentrated in vacuo to remove ethanol and the resulting aqueous solution was washed with 2×20 ml ethyl acetate. The aqueous layer was made basic with 10N sodium hydroxide and extracted with 3×75 ml ethyl acetate. The extract was washed with 20 ml water and brine, dried, and the solvent was removed in vacuo to give 1.87 g (77%) product as an oil.

WORKUP

后处理

  1. temperatureat reflux for 42 hours
  2. temperaturethe solution was heated
  3. temperatureat reflux for 6 hours
  4. concentrationThe cooled solution was concentrated in vacuo
  5. customto remove ethanol
  6. washthe resulting aqueous solution was washed with 2×20 ml ethyl acetate
  7. extractionextracted with 3×75 ml ethyl acetate
  8. washThe extract was washed with 20 ml water and brine
  9. customdried
  10. customthe solvent was removed in vacuo