Lithium Carbonate → HCID 68675630, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 3.0 g of the product of Step B, 7.41 g of 1-bromo-3,3-dimethyl-2-butanone, and 4.15 g of lithium carbonate in a 2:1 mixture of acetonitrile/DMF (90 mL) was heated at 100° C. for four h. The reaction mixture was cooled to room temperature, diluted with EtOAc, and washed with sat. ammonium chloride solution. The aqueous layer was extracted with EtOAc and the combined organic layers were washed with sat. lithium chloride solution, dried over sodium sulfate, filtered, and concentrated. Purification by silica gel chromatography afforded 1-tert-butyl-4-(3,3-dimethyl-2-oxo-butyl)-5-oxo-4,5-dihydro-1H-[1,2,4]triazole-3-carboxylic acid ethyl ester as a yellow oil. MS (M+H+)=312.3.

Provenance & Evidence