1-Bromo-3-methylbutan-2-one → HCID 57666787, compound

Participants

Reaction Conditions

Reaction Steps

2-Nitro-4-trifluoromethyl-thiobenzamide (55), (100 mg, 0.4 mmol) was dissolved in dioxan (4 ml) in a 10 ml test tube and to this solution was added 1-bromo-3-methyl-butan-2-one (52) (72.6 mg, 0.44 mmol). A stirrbar was added and the tube was sealed and heated to 100° C. over night. After cooling to ambient temperature, the vessel was de-capped, the solvent removed in vacuo and the residue partitioned between DCM and 10% aqueous NaHCO3 solution. The organic phase was separated and washed with additional 10% aqueous NaHCO3 solution and brine. The organic phase was filtered through a hydrophobic frit and the solvent removed in vacuo which gave the target compound (120 mg, 90%). LC/MS: (Method I): tR=2.26 min, >90%, m/z (ESI)=317 (MH+).

Provenance & Evidence