Ammonia → N-(6-chloro-7H-purin-2-yl)acetamide

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

45.0 g (0.27 mol) of tetraethylammonium chloride and 22.8 g (0.2 mol) of N-ethylpiperidine are added to a suspension of 42.6 g (0.18 mol) of 2,9-diacetylguanine in 450 ml of acetonitrile. 165.3 g (1.08 mol) of phosphorus oxychloride are then metered in at a temperature of 0° C. to 5° C. of the reaction mixture. The mixture is stirred at 25° C. for 20 hours, then introduced into 1.25 l of water such that 15° C. is not exceeded and the pH is at the same time kept between 4.8 and 5.5 using 12% strength ammonia solution. The mixture is stirred at 0° C. to 5° C. for 1 hour at a constant pH of 5, then the product is filtered off, washed with water and dried in vacuo at 50° C. 34.1 g of 2-acetamido-6-chloropurine are obtained. The final product is determined with the aid of HPLC on an RP-18 column in a reaction mixture of water, acetonitrile and acetic acid in the ratio 6:1:0.5.

Herkunft & Nachweise