反应详情

Under N2, to a solution of the product of Example 5J (122 mg, 0.5 mmol) in THF (anhydrous, 5 mL) was slowly added the solution of acetic acid (36 uL, 0.6 mmol) in THF (0.6 mL). The mixture was then stirred at ambient temperature for 6 h. White solid started to precipitate. The solid was then filtered and dried (110 mg, yield, 72%). M.p. 160-164° C. Solubility: 13.4 mg/mL (water). 1H NMR (CD3OD, 300 MHZ) δ 1.91 (s, 3H), 3.08 (dd, J=10.5, 6.4 Hz, 1H), 3.13 (dd, J=12.2, 4.8 Hz, 1H), 3.43-3.52 (m, 1H), 3.58 (dd, J=10.5, 4.8 Hz, 1H), 3.87 (d, J=10.5 Hz, 1H), 4.01 (d, J=11.8 Hz, 1H), 4.14 (dd, J=10.5, 8.5 Hz, 1H), 4.91 (dd, J=7.1, 4.7 Hz, 1H), 7.49 (d, J=2.7 Hz, 1H), 7.93 (d, J=2.7 Hz, 1H) ppm. MS (DCI/NH3) m/z 244 (M+H)+, 246 (M+H)+.

1. customto precipitate
2. filtrationThe solid was then filtered
3. customdried
4. custom(110 mg, yield, 72%)