Ammonium thiocyanate → HCID 59627506, compound

Participants

Reaction Steps

3-Chloro-3-oxo-propanoic acid ethyl ester (5 g; 33.2 mmol) was slowly added to a stirred solution of thiocyanic acid, ammonium salt (1:1) (2.781 g; 36.5 mmol) in CH3CN (110 ml) at room temperature. After 2 hours, 4-fluoro-3-(trifluoromethyl)benzenamine (4.27 ml; 33.2 mmol) was added. The solvent was removed under reduced pressure. The resulting residue partitioned between H2O/DCM and the phases separated. The aqueous phase was extracted with DCM (×2) and the combined organic extracts were washed with brine, dried and filtered. Yield: 3.656 g of intermediate D15.

Provenance & Evidence