反应详情

To a stirred solution of Intermediate 348H (0.43 g, 0.989 mmol) in DCM (8.0 mL) was added TFA (4.0 mL, 51.9 mmol) and the resulting solution was stirred at RT for 2 h. The reaction mixture was concentrated and the residue was extracted with DCM (10 mL), and washed successively with water, a saturated aq. NaHCO3 solution and brine. The organic layer was dried over Na2SO4, filtered and the filtrate concentrated under reduced pressure to afford Intermediate 3481 as an off-white solid (0.3 g, 67%). MS(ES): m/z=335 [M+H]+; 1H NMR (400 MHz, DMSO-d6) δ ppm 7.80-7.91 (m, 1H), 7.64-7.70 (m, 1H), 7.35-7.50 (m, 1H), 7.02-7.29 (m, 2H), 4.12-4.25 (m, 2H), 3.93 (d, J=16.56 Hz, 1H), 3.68-3.81 (m, 2H), 2.40 (br. s., 1H), 0.82-0.98 (m, 1H), 0.48 (d, J=8.03 Hz, 2H), 0.37 (d, J=5.02 Hz, 2H).

1. concentrationThe reaction mixture was concentrated
2. extractionthe residue was extracted with DCM (10 mL)
3. washwashed successively with water
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationthe filtrate concentrated under reduced pressure