Hydrochloric Acid → HCID 86696272, compound

Participants

Reaction Steps

To the solution of (76.2) (90 mg, 0.160 mmol) in THF (2 ml) was added about 2 N HCl (1 mL) at rt and the mixture was continue stirred for 30 mins, Checked the reaction by LCMS and TLC. The reaction solution was neutralized with sat.NaHCO3 aqueous until the pH to 8˜9 and extracted with DCM for three times, the combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated to give crude product which was purified by flash chromatography and eluented with DCM/MeOH (40:1˜20:1) to obtained pure desired product (76.3) as yellow solid (42 mg, yield 62.5%). 1H-NMR (400 MHz, MeOH-d4) δ ppm 8.95 (s, 1H), 8.72 (s, 1H), 7.98 (d, 1H), 7.87 (d, 1H), 7.80 (d, 1H), 7.75 (s, 1H), 7.39-7.43 (m, 2H), 3.78-3.84 (m, 1H), 3.68-3.74 (m, 2H), 3.02-3.08 (m, 2H), 2.57 (s, 3H), 1.98-2.01 (m, 2H), 1.62-1.71 (m, 2H). LCMS (method A): [M+H]+=420.1, tR=2.013 min.

Provenance & Evidence