Sodium Bicarbonate → HCID 86637508, compound

Participants

Reaction Steps

A solution of 0.98 g (0.0037 mole) of 2,2-difluoro-3-(2-thiophen-2-yl-ethylamino)-propionic acid ethyl ester in 1 mL of ethyl acetate was added over 5 minutes to a cooled (0 degrees) mixture of 0.72 g (0.0037 mole) of 2,4-dichloro-5-nitro-pyrimidine, 1.3 g (0.15 mole) of sodium bicarbonate and 10 mL of ethyl acetate. The cooling bath was removed and the mixture stirred for 17 hours at room temperature. Activated charcoal was added and after stirring briefly, the mixture was filtered through a pad of Celite, washing the filter pad with ethyl acetate. The filtrate was concentrated under reduced pressure to give 1.53 g of 3-[(2-chloro-5-nitro-pyrimidin-4-yl)-(2-thiophen-2-yl-ethyl)-amino]-2,2-difluoro-propionic acid ethyl ester (IV-269) as a yellow thick oil. This material was used directly in the next step without further purification.

Provenance & Evidence