HRID1576257

反应详情

EQUATION

反应方程式

HRID 1576257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9,9-di(2-methanesulphonyloxyethyl)-4-methoxy-9,10-dihydroanthracene (1.5 g.) and allylamine (7.0 g.) in n-propanol (30 ml.) is heated under reflux for 18 hours. The solvent is evaporated and 2N sodium hydroxide (20 ml.) is added; the suspension is extracted with ether and the ether layer washed with water, and extracted with 2N hydrochloric acid. The acid extract is washed with ether, basified with 15N ammonia solution, and the precipitated product is extracted into ether, the ether is washed with water and with brine, dried (MgSO4) and evaporated to give 1'-allyl-4-methoxy-9,10-dihydroanthracene-9-spiro-4'-piperidine as an oil.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 18 hours
  3. customThe solvent is evaporated
  4. addition2N sodium hydroxide (20 ml.) is added
  5. extractionthe suspension is extracted with ether
  6. washthe ether layer washed with water
  7. extractionextracted with 2N hydrochloric acid
  8. extractionThe acid extract
  9. washis washed with ether
  10. extractionthe precipitated product is extracted into ether
  11. washthe ether is washed with water and with brine
  12. dry with materialdried (MgSO4)
  13. customevaporated