反应详情

To a solution of Intermediate 1 (2.2 g, 10 mmol) in THF (3 mL) was added LiOH (10.8 mg, 0.451 mmol) and the reaction mixture was stirred at rt for 16 h. The reaction mixture was acidified to pH=1 using HCl (1M aq., 12.50 mL, 12.50 mmol) concentrated and then evaporated to dryness to provide Intermediate 6 (1.9 g, 10 mmol, 100% yield) as a gray solid. HPLC/MS (Method D) RT=0.42 min, [M+1]+ 184. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.28 (1H, d, J=7.1 Hz), 5.97 (1H, d, J=6.6 Hz), 3.62 (3H, s), 3.31 (3H, s).

1. concentrationconcentrated
2. customevaporated to dryness