Hydrochloric Acid → HCID 67021570, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1.5 g of 2-chloro-3-nitro-pyridine, 3.39 g of (4-amino-2-methyl-phenyl)-acetic acid methyl ester and 6.9 ml of an 4 N solution of HCl in dioxane in 30 ml of MeOH/dioxane (1:1, v/v) is stirred for 54 hours at 100° C. The mixture obtained is allowed to cool to rt and concentrated in vacuo. The concentrate obtained is dissolved in EtOAc, the mixture obtained is washed with a saturated aqueous solution of NaHCO3, dried (Na2SO4), filtered and concentrated. The concentrate obtained is subjected to silica gel column chromatography. [2-Methyl-4-(3-nitro-pyridin-2-ylamino)-phenyl]-acetic acid methyl ester is obtained. ES-MS: 302.1 [M+H]+; tR=4.79 min (System 1); Rf=0.43 (CH2Cl2).

Provenance & Evidence