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3
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2
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4
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1
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.024 mol) were added to the reaction vessel of the
(
0
5
(b) Doran, W. J. Med. Chem. 1959, 4, 1; (c) Bobranski, B.
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microwave reactor (Synthewave 402 monomode reactor
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wave irradiation, 40% power at 60 °C, for 7 min. The
automatic mode stirrer assisted in mixing and uniform
heating of the reactants. The reaction vessel was cooled to
room temperature. The small amount of acetic acid
produced was removed under reduced pressure and to the
residue was added ethanol (10 ml). The resulting light
yellow solid was filtered off and recrystallized from
ethanol as a white crystalline solid (1.45 g, 78%), mp
6
7
8
9
. (a) Gauri, K. K.; Kohlage, H. Chemotherapy 1969, 14,
1
59–170; (b) Gauri, K. K.; Rohde, B. Klin. Wochenschr.
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1
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1
996; Vol. 7, pp 397–429.
(
121–122 °C).
0. Equimolar amounts of N,N-dimethylurea 2a (1.10 g,
.0125 mol) and cyanoacetic acid 5 (1.06 g, 0.0125 mol)
were thoroughly mixed and then acetic anhydride 3
1.275 g, 0.025 mol) was added to the reaction vessel of
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2
0
(
1
1
1
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the microwave reactor. The reaction mixture was
exposed to microwave irradiation at 40% power for
1
reaction vessel was cooled to room temperature and
ethanol (5 ml) added. A 5% NaOH solution (6 ml) was
added with stirring whereby N,N-dimethyl-6-amino-
uracil 6a precipitated. The white solid compound was
collected by filtration and recrystallized from water as
a white crystalline solid (1.54 g, 80%), mp (291–
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0 min keeping the temperature below 60 °C. The
1
1
2
93 °C).