反应详情

A mixture of diethyl 2-(2,4,6-trifluorophenyl)malonate (U.S. Pat. No. 6,156,925) (870 mg, 3.0 mmol), 2-aminoimidazole (Hel. Acta. Chim. 76, 2066 (1993)) (274 mg, 3.3 mmol), and 1.0 mL of tributylamine is stirred under nitrogen atmosphere at 160° C. for 0.5 h and cooled to room temperature. The mixture is dissolved in ethyl acetate and the organic layer is washed with 1.0 N hydrochloric acide (×3) and saturated sodium chloride, dried over magnesium sulfate, and concentrated. The residue is dissolved in ethyl acetate (5 mL) and to this solution is added hexanes (50 mL). The precipitates are collected by filtration, washed with hexanes to give 6-(2,4,6-trifluorophenyl)imidazo[1,2-a]pyrimidine-5,7-diol as a tan solid (180 mg). MS: m/z 279.9(M−H).

1. washthe organic layer is washed with 1.0 N hydrochloric acide (×3) and saturated sodium chloride
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated
4. dissolutionThe residue is dissolved in ethyl acetate (5 mL) and to this solution
5. additionis added hexanes (50 mL)
6. filtrationThe precipitates are collected by filtration
7. washwashed with hexanes