反应详情

温度

60 °C

To a stirred solution of N-dodecyl-3,5-bis(3-chlorophenyl)-4-(2-hydroxyethoxy)benzamide (Example 1, Step 2), (0.866 g, 1.52 mmol) in THF (8 mL) was added NaH (0.10 g, 80%, 3.34 mmol). The mixture was stirred at 60° C. for 50 min and was then cooled to room temperature. Methyl bromoacetate (0.158 mL, 2.67 mmol) was added and the mixture was stirred at 60° C. overnight. The reaction was cooled, quenched with 1.0 N HCl, and extracted with ethyl acetate. The organic phase was dried (MgSO4) and concentrated. Crude product was purified by HPLC. Yield: 0.177 g (18%) of product as an oil. 1H NMR (CDCl2) δ 7.72 (s, 2H), 7.63 (s, 2H), 7.50 (m, 2H), 7.39 (m, 4H), 6.20 (t, 1H), 3.78 (m, 5H), 3.49 (m, 4H), 3.31 (m, 2H), 1.68 (m, 2H), 1.30 (m, 18H), 0.88 (t, 3H).

1. temperaturewas then cooled to room temperature
2. stirringthe mixture was stirred at 60° C. overnight
3. temperatureThe reaction was cooled
4. customquenched with 1.0 N HCl
5. extractionextracted with ethyl acetate
6. dry with materialThe organic phase was dried (MgSO4)
7. concentrationconcentrated
8. customCrude product was purified by HPLC