反应详情

To a solution of Compound 252 (150 mg, 0.37 mmol) in dry THF (3 mL) was added cyclopropylcarbonyl chloride (34 μL, 0.37 mmol) at 0° C. Slowly the temperature was raised to room temperature and stirred for an additional hour. Reaction was quenched with aqueous NaHCO3 solution and extracted with EtOAc, washed with brine, dried over Na2SO4 and finally purified preparative HPLC to provide Compound 253 (132 mg, 75%). 1H NMR (400 MHz, DMSO-d6) δ ppm 0.63 (br. d, J=8.1 Hz, 2H) 0.80 (br. s., 2H) 1.18 (t, J=7.45 Hz, 3H) 1.48 (td, J=8.02, 3.92 Hz, 1H) 2.27 (s, 3H) 3.26 (s, 3H) 3.41 (q, J=7.45 Hz, 2H) 3.98 (s, 3H) 7.17 (s, 1H) 7.54 (s, 1H) 7.88 (t, J=7.71 Hz, 1H) 8.04 (d, J=8.08 Hz, 2H) 8.14 (s, 1H) 8.31 (d, J=1.26 Hz, 1H) 12.31 (s, 1H); [M+H] calc'd for C26H28N3O4S, 478.2; found, 478.3.

1. customReaction
2. customwas quenched with aqueous NaHCO3 solution
3. extractionextracted with EtOAc
4. washwashed with brine
5. dry with materialdried over Na2SO4 and finally purified preparative HPLC