反应详情

4,5-Diamino-6-hydroxypyrimidine (527 mg, 4.18 mmol) was added to an aqueous suspension of sodium hydrogen carbonate (3.15 g, 41.8 mmol) in water (10 mL) under cooling with ice. Subsequently, a solution of 4-isobutoxy-3-nitrobenzoyl chloride (1.08 g, 4.18 mmol) in ethyl acetate (10 mL) was added. The resulting mixture was stirred for 3 hours under cooling with ice, made acetic by addition of 6 M hydrochloric acid, placed under reduced pressure at room temperature to distill ethyl acetate off, and stirred for 30 min. at room temperature. The precipitated solid product was collected by filtration, washed successively with water and diethyl ether, and dried successively in air and reduced pressure, to give 963 mg (yield 69%) of the desired compound in the form of a powdery product.

1. temperatureunder cooling with ice
2. temperatureunder cooling with ice
3. customplaced under reduced pressure at room temperature
4. distillationto distill ethyl acetate off, and
5. stirringstirred for 30 min. at room temperature
6. filtrationThe precipitated solid product was collected by filtration
7. washwashed successively with water and diethyl ether
8. customdried successively in air and reduced pressure