Ammonium Hydroxide → HCID 23321130, compound

Participants

Reaction Steps

A mixture of 5-(2-allyl-3-hydroxy-4,5-dimethoxybenzyl)-2,4-diaminopyrimidine (1.50 g, 4.74 mmol) and polyphosphoric acid (50 g) was heated to 95° and maintained at this temperature with stirring until a clear pale yellow syrup was achieved (about 1 h). This syrup was poured into ice-water and the resulting solution basified with ammonium hydroxide. The resulting white solid (1.3 g) was chromatographed on silica gel eluted with MeOH:CH2Cl2 /1:9 to give the title compound as white powder (1.2 g). Recrystallization from 95% ethanol gave clusters of white needles, mp 216°-219°. Anal. Calcd for C16H20N4O3 (316.37); C, 60.74; H, 6.37; N, 17.71. Found: C, 60.48; H, 6.41; N, 17.63.

Provenance & Evidence