Dimethyl Sulfoxide → HCID 58674272, compound

Participants

Reaction Steps

Under argon, 30.8 mg (0.15 mmol) N-(3,5-dichlorophenyl)urea are stirred together with 39.3 mg (0.3 mmol) 4-formylbenzonitrile, 39 mg (0.3 mmol) ethyl 3-oxo-butanoate and 90 mg trimethylsilylpolyphosphate in 0.5 ml dioxan at 80° C. for 4 hours. After adding a small amount of DMSO, the reaction mixture is filtered and purified by preparative HPLC (column: Agilent Zorbax Extend C18 20 mm×50 mm, 5 μm; solvent A: acetonitrile, solvent B: water+0.1% conc. aq. ammonia; gradient: 0 min 10% A, 2 min 10% A, 6 min 90% A, 7 min 90% A, 7.1 min 10% A, 8 min 10% A; flow rate 25 ml/min; wavelength: 220 nm; injection volume: approx. 500 μl; number of injections: 1). The product containing fractions are combined and concentrated in vacuo.

Provenance & Evidence