Dimethylformamide → HCID 178454934, compound

Participants

Reaction Steps

To a suspension of sodium hydride (34 mg, 0.86 mmol) in N,N-dimethylformamide (1 mL) was added a N,N-dimethylformamide solution of N-[2-amino-5-(tert-butylthio)pheny]-2,2-dimethylpropanamide (Step C, 200 mg, 0.71 mmol) at room temperature. After stirring for 30 min, a N,N-dimethylformamide solution of 1,6-dioxaspiro[2,5]octane (Phosphorus and Sulfur and the Related Elements 1984, 19, 113-129., 98 mg, 0.86 mmol) was added. The mixture was stirred at room temperature for 3 h and at 100° C. for 5 h. Water (10 mL) was added and the mixture was extracted with ethyl acetate (15 mL). The organic extract was washed with water (5 mL) and brine (5 mL) and concentrated. The residue was purified by pTLC (ethyl acetate:hexane=1:2 as eluent) to afford the title compound as pale brown oil.

Provenance & Evidence