m-Tolyl isocyanate → HCID 20097077, compound

Participants

Reaction Steps

The procedure is analogous to that described in Example 1, but 3.8 g of 2-(2-amino-N-phenylacetamido)-N-(3,4-difluorophenyl)-N-methylacetamide and 1.4 g of 3-methylphenyl isocyanate are used as the starting material. The crude product obtained is purified by chromatography on 80 g of silica (0.065-0.200 mm) contained in a column 2.5 cm in diameter [eluent: ethyl acetate/cyclohexane (75-25 by volume)], collecting 20 cm3 fractions. Fractions 3 to 8 are combined and concentrated to dryness under reduced pressure (2.7 kPa) at 40° C. After recrystallization from a cyclohexane/ethyl acetate mixture (50-50 by volume), 0.5 g of N-(3,4-difluorophenyl)-N-methyl-2-{2-[3-(3-methylphenyl)ureido]-N-phenylacetamido}acetamide melting at 163° C is obtained.

Provenance & Evidence