反应详情

Add 6-amino-3-methyl-5-(phenylmethyleneamino )pyrimidine-2,4-dione (85 g=0.35 mol) to CH2Cl2 (1.6L) and MeOH (1.6L). Stir the suspension, add HOAc (21.9 ml=0.35 mol), then NaCNBH3 (21.9 g=0.35 mol). Stir 1.5 hr, and add HOAc (2 ml) and NaCNBH3 (2.0 g). After another 30 min, concentrate to ca. 1.6L on a rotovap (35° C. bath). Chill the crystalline mixture, filter, and wash with cold MeOH. Stir the product 15 min in 0.5L boiling MeOH, chill, filter, and dry to obtain the title compound, m.p. 206°-218° C.

1. stirringStir 1.5 hr
2. concentrationconcentrate to ca. 1.6L on a rotovap (35° C. bath)
3. temperatureChill the crystalline mixture
4. filtrationfilter
5. washwash with cold MeOH
6. stirringStir the product 15 min in 0.5L
7. temperaturechill
8. filtrationfilter
9. customdry