反应详情

To a solution of compound 3 (100 mg, 0.21 mmol) in CH2Cl2 (3 mL) under inert atmosphere was added NCS (58 mg, 0.43 mmol) at RT and stirred for 16 h. The reaction mixture was diluted with water (10 mL) and extracted with CH2Cl2 (2×15 mL). The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure to obtain the crude. The crude was purified (silica gel; 14-17% EtOAc/Hexanes) to afford 5 (35 mg, 33%) as an off-white solid. 1H NMR (400 MHz, CDCl3): δ 7.71-7.66 (m, 3H), 7.30 (d, J=7.6 Hz, 1H), 7.19 (dd, J=8.8, 6.4 Hz, 1H), 7.04-6.97 (m, 2H), 4.40 (q, J=7.2 Hz, 2H), 4.27 (q, J=7.6 Hz, 2H), 1.58 (t, J=7.6 Hz, 3H), 1.49 (t, J=7.2 Hz, 3H); LC-MS (ESI): m/z 496.7 (M+H+).

1. extractionextracted with CH2Cl2 (2×15 mL)
2. dry with materialThe combined organic extracts were dried over Na2SO4
3. concentrationconcentrated under reduced pressure
4. customto obtain the crude
5. customThe crude was purified (silica gel; 14-17% EtOAc/Hexanes)