反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
8-Ethyl-4-methyl-2-(methylsulfonyl)-6-phenylpyrido[2,3-d]pyrimidin-7(8H)-one (275 mg, 0.80 mmol) and 4-(4-ethylpiperazin-1-yl)aniline (197 mg, 1.2 equiv.) were added to dimethyl sulfoxide (5 mL) and the resulting mixture was heated to 100° C. and stirred overnight. After cooling to room temperature, the reaction was partitioned between aqueous and organic layers with ethyl acetate and H2O, organic layer was dried with anhydrous magnesium sulfate, filtered and evaporated, and directly applied to prep-LC to provide the title compound in (210.0 mg, 56% yield): 1H NMR (400 MHz, CDCl3): δ 7.80 (s, 1H), 7.62 (d, 2H), 7.60 (d, 2H), 7.40 (m, 2H), 7.18 (s, 1H), 6.95 (d, 2H), 4.50 (q, 2H), 3.22 (m, 4H), 2.70 (m, 4H), 2.60 (s, 3H), 2.50 (m, 2H), 1.40 (t, 3H), 1.20 (t, 3H); MS (EI) for C28H32N6O: 469.10 (MH+).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customthe reaction was partitioned between aqueous and organic layers with ethyl acetate and H2O, organic layer
- dry with materialwas dried with anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated