m-Tolyl isocyanate → HCID 14996911, compound

Participants

Reaction Steps

The procedure is analogous to that described in Example 1, but 1.4 g of tert-butyl N-{2-[(2-aminoacetyl)phenylamino]acetyl}-N-phenylglycinate and 0.45 g of 3-methylphenyl isocyanate are used as the starting material. The product obtained is purified by chromatography on 80 g of silica (0.04-0.063 mm) contained in a column 3 cm in diameter [eluent: methylene chloride/methanol (98-2 by volume)] using an excess pressure of 30 kPa of nitrogen and collecting 35 cm3 fractions. Fractions 19 to 21 are combined and concentrated to dryness under reduced pressure (2.7 kPa) at 40° C. After churning the residue obtained with 25 cm3 of heptane, 0.4 g of tert-butyl N-{2-{2-[3-(3-methylphenyl)ureido]-N-phenylacetamido}acetyl}-N-phenylglycinate melting at 76°-80° C. is obtained.

Provenance & Evidence