4-Isothiocyanato-2-(trifluoromethyl)benzonitrile → HCID 86668136, compound

Participants

Reaction Conditions

Reaction Steps

Compound 8 was prepared according to General Method 3. A mixture of sodium 2-(4-(2-(dimethylamino)ethoxy)phenylamino)-2-methylpropanoate (107 mg, 0.37 mmol) and 2-(trifluoromethyl)-4-isothiocyanatobenzonitrile (107 mg, 0.44 mmol) was heated at 100° C. for 1 h then 82° C. for 12 h. The crude product was purified by silica gel chromatography using 100-200 Mesh silica gel (10% methanol in DCM) to obtain 30 mg of 4-(3-(4-(2-(dimethylamino)ethoxy)phenyl)-4,4-dimethyl-5-oxo-2-thioxoimidazolidin-1-yl)-2-(trifluoromethyl)benzonitrile. The product was converted its HCl salt by treating with ethanolic HCl, HPLC, Column: HYPERSIL GOLD C18, 4.6×250 mm, 5 μm, Mobile Phase A: 0.05% TFA, Mobile Phase B: ACN, Gradient: 10% to 90% B in 10 min, hold for 10 min. 90% to 10% B in 1 min, Flow Rate: 1 mL/min, Retention time: 9.568 min, M+1, 477.

Provenance & Evidence