反应详情

To a solution of 1 gm Hg2Cl2 in 30 ml H2O was added 1 ml of concentrated HCl followed by 24 gms powdered Zn (portion wise) with mechanical stirring. The resulting mixture was stirred together for 5 minutes, then the liquid phase was decanted off, and 15 ml H2O was added, followed by 36 ml concentrated HCl. This mixture was cooled to room temperature (the reaction to this point is exothermic), then 5.4 gms 11-benzoylundecanoic acid was added followed by 25 ml toluene. The resulting mixture was stirred and refluxed for 20 hours; 12 ml concentrated HCl was added during the first 6 hours of the reflux. The reaction mixture was cooled, the liquid was decanted, the phases were separated and the solid was three times triturated with 25 ml ether. The aqueous phase was 3×15 ml ether extracted; all organic phases were combined, washed with water and brine and dried over MgSO4. The drying agent was filtered off, and the solvents were removed in vacuo to give a solid residue. This residue was dissolved in ether, extracted with dilute NaOH, and the organic layer was discarded. The aqueous layer was acidified with concentrated HCl, then extracted with ether. This ether solution was washed with water and brine, dried over MgSO4, filtered, and evaporated in vacuo to give 4.2 gms title product which was used without further purification.

1. customthe liquid phase was decanted off
2. addition15 ml H2O was added
3. customthe reaction to this point
4. additionwas added
5. stirringThe resulting mixture was stirred
6. temperaturerefluxed for 20 hours
7. temperatureThe reaction mixture was cooled
8. customthe liquid was decanted
9. customthe phases were separated
10. customtriturated with 25 ml ether
11. extractionextracted
12. washwashed with water and brine
13. dry with materialdried over MgSO4
14. filtrationThe drying agent was filtered off
15. customthe solvents were removed in vacuo
16. customto give a solid residue
17. extractionextracted with dilute NaOH
18. extractionextracted with ether
19. washThis ether solution was washed with water and brine
20. dry with materialdried over MgSO4
21. filtrationfiltered
22. customevaporated in vacuo