Hydrochloric Acid → HCID 86747732, compound

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Reaction Steps

A solution of N-{N'-(tert-butoxycarbonyl)-4-[bis(2-chloroethyl)amino]-(L)-phenylalanyl}-5-amino-1-hydroxypentane-1,1-diphosphonic acid trisodium salt (35 mg) in methanol saturated with hydrochloric acid (2 ml) is heated to 40°-50° C. for 4 hours, then the solution is concentrated to reduced volume and the precipitated sodium chloride is filtered. The filtrate is evaporated to dryness and the residue is triturated with acetone and filtered. After recrystallization from ethanol/ethyl ether, N-{4-[bis(2-chloroethyl)amino]-(L)-phenylalanyl}-5-amino-1-hydroxypentane-1,1-diphosphonic acid monohydrochloride (25 mg) is obtained, m.p. >260° C., [α]D =+7.9 (c=2, methanol), NMR (TMS, D2O): 1.25÷1.40 (m, 2H), 1.42÷1.72 (m, 2H); 1.8÷2.06 (m, 2H); 2.9÷3.2 (m, 4H); 3.65 (t, 4H); 4.0 (t, 4H); 4.1 (t, 1H); 7.35 (s, 4H).

Provenance & Evidence