Phosphate → Dihydro-1-[3-(hexyloxy)phenyl]-1,2,4-triazine-3,5-(2H,4H)-dione

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Reaction Steps

Sodium methoxide (0.33 g, 6.2 mmol) was added under nitrogen to a stirred solution of the urea (Intermediate 70, 1.00 g, 3.1 mmol) in 1,2-dimethoxyethane (25 ml) over 4 A° molecular sieves. After 15 minutes the mixture was poured into pH6.5 aqueous phosphate buffer (100 ml) and extracted with ethyl acetate (3×100 ml). The combined extracts were dried (MgSO4) and evaporated to afford the crude product as an off-white solid. Trituration with hexane/ether (ca. 1:2) (25 ml) gave the title compound as a white powder (600 mg, 67%) m.p. 161°-163° C.

Provenance & Evidence