Reaction #2977852
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04448960
Conditions: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: 10.5 g (0.105 mole) of triethylamine are added to a solution of 15.4 g (0.1 mole) of 6-methyl-9-oxo-1,5-diazabicyclo[4.3.0]nonane in 100 ml of toluene. The mixture is cooled to -10° C. and 14.8 g (0.1 mole) of dichloroacetyl chloride are added dropwise at from -10° to -5° C. The batch is stirred for a further 4 hours and the triethylamine hydrochloride which has precipitated is filtered off. After evaporating the toluene from the filtrate, crystals separate out, and these can be recrystallized from a 1:3 toluene/acetone mixture. 17.7 g of 5-dichloroacetyl-6-methyl-9-oxo-1,5-diazabicyclo[4.3.0]nonane, a melting point 144°-147° C., are obtained. the triethylamine hydrochloride which has precipitated is filtered off After evaporating the toluene from the filtrate, crystals separate out these can be recrystallized from a 1:3 toluene/acetone mixture
Source ID: ord-c6a8a21c8676430ca8e8cd53b98dbeb4