反应详情

A solution of above crude product 40 (220 mg, purity 57% 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 43 (Example 7) as a white solid (35.7 mg). (ES, m/z): 245.0. 1H NMR (300 MHz, D2O) δ 6.20-6.22 (d, J=6.3 Hz, 1H), 5.79-5.87 (m, 1H), 5.30-5.38 (m, 2H), 3.98-4.08 (m, 2H), 3.87-3.91 (t, J=6.0 Hz, 1H), 3.46-3.52 (m, 1H), 2.93 (s, 6H).

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