反应详情

温度

28 °C

To a solution of 4-chloro-5,6-diphenyl-2-(trifluoromethyl)pyrimidine (0.5 g, 1.49 mmol, prepared according to the procedure described in PCT/IB03/02879) in dimethylformamide (5 ml) was added 1-pyridin-2-yl piperazine (0.107 g, 0.66 mmol) and anhydrous potassium carbonate (0.2 g) under stirring at 28° C. The reaction mixture was stirred for 4 hours and when TLC conformed the completion, it was poured onto ice. The solid thus obtained was filtered and washed with water (20 ml). The above solid was then dissolved in dichloromethane (50 ml) and dried over anhydrous sodium sulphate. Evaporation of the solvent afforded the title compound (0.48 g, yield 69.66%, purity by HPLC 99.8%). m.p. 165-167° C. 1H-NMR (CDCl3) δ: 3.43 (s, 8H), 6.58-6.64 (m, 2H), 7.14-7.21 (m, 7H), 7.26-7.29 (m, 3H), 7.45-7.49 (t, 1H), 8.14-8.15 (d, 1H). IR cm−1 (KBr): 3436, 2839, 1591, and 1557. MS m/z: 462.1 (M++1).

1. stirringThe reaction mixture was stirred for 4 hours
2. additionwas poured onto ice
3. customThe solid thus obtained
4. filtrationwas filtered
5. washwashed with water (20 ml)
6. dissolutionThe above solid was then dissolved in dichloromethane (50 ml)
7. dry with materialdried over anhydrous sodium sulphate
8. customEvaporation of the solvent