反应详情

A solution of above crude product 41 (260 mg, purity 54% by LC-MS) in dichloromethane (10 mL) was treated with TFA (1 mL) for 4 hours at room temperature. The solution was adjusted to pH at 8 with NH4OH, and then condensed to give a crude product, which was purified by Prep-HPLC with the following conditions (Agilent 1200 prep HPLC: Column, SunFire Prep C18,19*50 mm 5 um; mobile phase, WATER with 0.03% NH4OH and CH3CN (10% CH3CN up to 45% in 10 min; Detector, UV 220 nm) to provide compound 42 (Example 6) as a white solid (38 mg). (ES, m/z): [M+H]+ 247.0. 1H NMR (300 MHz, D2O) δ 6.18-6.21 (d, J=6.6 Hz, 1H), 4.09-4.13 (t, J=6.0 Hz, 1H), 3.91-3.94 (t, J=4.8 Hz, 1H), 3.42-3.44 (m, 2H), 2.92 (s, 6H), 1.69-1.77 (m, 1H), 1.40-1.50 (m, 1H), 0.84-0.89 (t, J=7.5 Hz, 3H).

1. customcondensed
2. customto give a crude product, which
3. customwas purified by Prep-HPLC with the following conditions (Agilent 1200 prep HPLC