Hydrochloric Acid → 1,6-Dichlorohexan-2-one

In 300 ml of ehter solution of diazomethane prepared from 43 g of p-tosyl-N-methyl-N-nitrosoacetamide was added under stirring 30 ml of ether solution of 8 g of 5-chlorovalerylchloride dropwise at -5° to 0° C., and the solution was allowed to stand at the same temperature for 2 hours. Hydrogen chloride gas was passed through the reaction solution at 0° C. and the solution was allowed to stand at the same temperature for 0.5 hours. To the solution was added 100 ml of water and the ether layer was separated. The aqueous layer was further extracted twice each time with 100 ml of ether. The ether layers were combined and the obtained ether solution was dried over anhydrous magnesium sulfate and the solvent was distilled away and the residue was distilled under reduced pressure to provide 8.2 g of 1,6-dichloro-2-hexanone showing a boiling point of 120° to 125° C. (14 mm Hg). ##STR51##

1. additionwas added
2. customwas passed through the reaction solution at 0° C.
3. waitto stand at the same temperature for 0.5 hours
4. customthe ether layer was separated
5. extractionThe aqueous layer was further extracted twice each time with 100 ml of ether
6. dry with materialthe obtained ether solution was dried over anhydrous magnesium sulfate
7. distillationthe solvent was distilled away
8. distillationthe residue was distilled under reduced pressure

ORD record

ord-fdebbc2044294a54aea7eca2f263b519

Source dataset

uspto-grants-1982_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04362736