Ammonium Chloride → HCID 57514209, compound

Participants

Reaction Conditions

Reaction Steps

1-(5-Bromo-2-fluorophenyl)-1-ethanone ([CAS 198477-89-3], 65 g, 299.5 mmol) and NH4Cl (32 g, 599 mmol) were dissolved in NH3 (in MeOH, 600 mL). Trimethylsilyl cyanide ([CAS 7677-24-9], 100 g, 1008.6 mmol) was added to the above mixture on an ice bath. The reaction mixture was stirred for 2 days at 30° C. The mixture was evaporated under reduced pressure. The residue was extracted with CH2Cl2 (2×300 mL). The organic layer was collected, dried and evaporated to give the crude product, which was purified by flash column chromatography over silica gel (gradient eluent:ethyl acetate/petrol ether from 1/20 to 1/2). The product fraction was collected and evaporated to give I-11 (60 g, 82%).

Provenance & Evidence