Water → HCID 20061258, compound

Participants

Reaction Steps

An oily substance obtained by dissolving 1.0 g of 6-(aziridin-1-yl)-1,3-dimethyl-5-nitro-2,4(1H,3H)-pyrimidinedione, 0.99 g of N-(2-hydroxethyl)-3-(4-nitrophenyl)propylamine and 50 mg of p-toluenesulfonic acid in 1.0 ml of dimethylformamide was allowed to react at 90° C. for 3 hours. The reaction mixture was cooled down to room temperature, added with 10 ml of water and then vigorously stirred. Crystals formed were collected by filtration, dissolved in chloroform and then subjected to silica gel chromatograph (chloroform/methanol=40:1 (v/v)) for purification. Thus, 0.44 g of 1,3-dimethyl-6-{2-[N-(2-hydroxyethyl)-3-(4-nitrophenyl)propylamino]ethylamino}-5-nitro-2,4(1H,3H)-pyrimidinedione (a free form of compound 180) was obtained.

Provenance & Evidence