反应详情

To a solution of compound 4e (195 mg, 0.46 mmol) in DCM (0.9 mL) was added ClSO3H (0.45 mL, 7.02 mmol) at −40° C. under Ar. The mixture was slowly warmed to rt and stirred for 48 h. To the mixture was added dropwise to NH3 (3N in THF, 20 mL) at −20° C. and the mixture was stirred for 2 h, evaporated, redissolved in water, extracted with EA, washed with brine, dried with Na2SO4, concentrated and purified by prep-HPLC to afford compound 4 (16 mg, 8%) as light yellow solid. 1H-NMR (400 MHz, CDCl3) δ: 8.28 (s, 1H), 7.49 (t, J=1.8 Hz, 1H), 7.33 (d, J=1.6 Hz, 2H), 5.71 (s, 2H), 2.88 (m, 4H), 2.57 (s, 3H), 1.35-1.27 (m, 24H). LC-MS (ESI+) m/z: 496.6 [M+1]+.

1. stirringthe mixture was stirred for 2 h
2. customevaporated
3. dissolutionredissolved in water
4. extractionextracted with EA
5. washwashed with brine
6. dry with materialdried with Na2SO4
7. concentrationconcentrated
8. custompurified by prep-HPLC