反应详情

A solution of 6.0 g. of 4-carbobenzoxypiperazine-2-carboxylic acid hydrochloride, 3.3 g. of 2-chloro-3-nitropyridine and 15 ml. of triethyl amine in 100 ml. of dimethyl sulfoxide is heated at 60° with stirring for 18 hours. The mixture is diluted with 400 ml. of water, acidified to pH 3 with concentrated hydrochloric acid, and extracted repeatedly with ether. The combined ether extracts are dried (MgSO4) and concentrated. The residue is crystallized from ethyl acetate/heptane to give 6.3 g. of the title product, m.p. 145°-147°.

1. additionThe mixture is diluted with 400 ml
2. extractionextracted repeatedly with ether
3. dry with materialThe combined ether extracts are dried (MgSO4)
4. concentrationconcentrated
5. customThe residue is crystallized from ethyl acetate/heptane
6. customto give 6.3 g