반응 #367189

반응 방정식

2,4-diamino-5-(3-hydroxy-4,5-dimethoxybenzyl)pyrimidine

L-(-)-malic acid

ammonium hydroxide

→

2,4-Diamino-5-(7,8-dimethoxy-2-oxo-2H-1-benzopyran-5-ylmethyl)pyrimidine

용매

반응 조건

후처리

1. 1
   온도was heated at 90°-100° for 4 hours
2. 2
   여과The title compound was filtered off
3. 3
   세척washed with ethanol
4. 4
   기타Yield

실험 절차

A mixture of 1.38 g (0.005 mole) of 2,4-diamino-5-(3-hydroxy-4,5-dimethoxybenzyl)pyrimidine and 1.01 g (0.0075 mole) of L-(-)-malic acid in polyphosphoric acid (30 g) was heated at 90°-100° for 4 hours. The resulting clear syrup was poured into ice-water (150 mL) and basified (pH 8) with conc'd ammonium hydroxide. The title compound was filtered off and washed with ethanol. Yield, 0.26 g (16%); m.p. 278°-280° dc; structure confirmed by 13C and 1H NMR and mass spectra. Anal. Calcd. for C16H18N4O3 : C, 58.53; H, 4.91; N, 17.07. Found: C, 58.27; H, 4.99; N, 16.97.

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