反应详情

温度

70 °C

A mixture of Example 294A (0.100 g, 0.229 mmol), (benzotriazol-1-yl-oxytripyrrolidinophosphonium hexafluorophosphate (0.143 g, 0.275 mmol), triethylamine (0.160 mL, 1.147 mmol), and azetidin-3-ol.hydrochloride (0.030 g, 0.275 mmol) in N,N-dimethylformamide (2.5 mL) was stirred for 3 hours and was treated slowly with water. The solid was filtered, washed with water, dried in a vacuum oven, heated in 6 mL ethyl acetate/heptanes (1:1) at 70° C. for 2 hours, filtered, washed with ethyl acetate/heptanes (1:1), and vacuum oven-dried to give the title compound. 1H NMR (500 MHz, Methanol-d4) δ 2.54-2.60 (m, 2H), 2.78 (t, J=5.7 Hz, 2H), 3.21 (d, J=2.9 Hz, 2H), 3.29 (d, J=3 Hz, 1H), 3.76 (s, 4H), 4.02-4.08 (m, 1H), 4.22 (dd, J=10.7, 6.8 Hz, 1H), 4.44-4.52 (m, 1H), 4.52-4.62 (m, 2H), 6.16 (s, 1H), 6.34-6.39 (m, 1H), 7.08-7.24 (m, 3H), 8.07 (d, J=2.8 Hz, 1H). MS (ESI+) m/z 455.0 (M+H)+.

1. filtrationThe solid was filtered
2. washwashed with water
3. customdried in a vacuum oven
4. filtrationfiltered
5. washwashed with ethyl acetate/heptanes (1:1), and vacuum
6. customoven-dried