Ammonium thiocyanate → HCID 59627520, compound

Participants

Reaction Steps

A mixture of thiocyanic acid, ammonium salt (5 g, 0.065 mol) in CH3CN (42 ml) was stirred for 15 min. at r.t. 4-Chloro-4-oxo-butanoic acid ethyl ester (0.061 mol) was added dropwise and the mixture was stirred for 30 min. at 60° C. The mixture was cooled to 0° C. and then 3,4-difluoroaniline (6 mL, 0.061 mol) was added dropwise. The reaction mixture was stirred for 30 min. at r.t. The mixture was then quenched with ice-water and stirred for 15 min. at 0° C. The mixture was filtered through a sinter funnel, dried and azeotroped with toluene to remove remaining water. Yield: 16.40 g of intermediate D5 (85%, yellow solid).

Provenance & Evidence