反应详情

温度

60 °C

A mixture of 3-3 (11.0 g) and 25 mL ethanolamine was stirred at 60° C. for 1 h. The reaction was then allowed to cool to room temperature, poured into ice-water (100 mL), and extracted with CH2Cl2 (3×100 mL). The combined organic layers were washed with brine (150 mL), dried over MgSO4, filtered, and concentrated in vacuo, giving 5.82 g of crude 3-4 as a viscous amber oil. 1H NMR (CDCl3, 300 MHz): 3.94 (br, 2H), 3.08 (m, 2H), 1.85 (m, 2H), 1.51 (m, 4H), 1.44 (s, 9H); MS (Electrospray): m/z 218.2 (M−Me+H), 177.2 (M−t−Bu+H).

1. temperatureto cool to room temperature
2. extractionextracted with CH2Cl2 (3×100 mL)
3. washThe combined organic layers were washed with brine (150 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo