Process for the manufacture of 5-dichloroacetyl-3,3,6-trimethyl-9-oxo-1,5-diazabicyclo4.3.0! nonane

US5677452A · kind A · utility

Assignee

• BASF SE

Inventors

• Gernot Reissenweber · Haßloch, DE
• Winfried Richarz · Riedstadt, DE
• Knut Koob · Mutterstadt, DE

Key dates

• Filing date: Oct 24, 1996
• Grant date: Oct 14, 1997
• Expiry date: Oct 24, 2016

Classification

• Technology area (CPC C): Chemistry; Metallurgy
• CPC primary: C07D487/04
• WIPO field: Organic fine chemistry
• WIPO sector: Chemistry

Abstract

The manufacture of 5-dichloroacetyl-3,3,6-trimethyl-9-oxo-1,5-diazabicyclo4.3.0!-nonane I by the reaction of 3,3,6-trimethyl-9-oxo-1,5-diaza-bicyclo4.3.0!nonane II with dichloroacetyl chloride in the presence of a solvent and a base, wherein PA0 a) this reaction is carried out in a two-phase system comprising a virtually water-insoluble organic solvent and water, and sodium or potassium hydroxide acting as the base is metered in at a rate corresponding to the rate of consumption of the dichloroacetyl chloride such that the aqueous phase exhibits a pH of from 7 to 9, and PA0 b) the resulting product is separated.