反应详情

A solution of the product from Step A above (150 mg, 0.28 mmol) in conc HCl/EtOH (1:2 mixture, 3 mL) was stirred for 2 h at room temperature. The reaction mixture was concentrated under vacuum and the residue was azeotroped twice with ethanol to give the desired product as an amorphous solid. API-MS: 433 (M+1). 1H NMR (300 MHz, d4-MeOH): d 8.0 (d, 2 H), 7.75 (d, 2 HO, 7.66 (d, 2 H), 7.4 (m), 4.0 (s, 3 H), 3.96 (s, 3 H)m 3.65 (t, 2 H), 3.28 (m, 2 H), 2.96 (t, 2 H), 2.0-1.2 (m).

1. concentrationThe reaction mixture was concentrated under vacuum
2. customthe residue was azeotroped twice with ethanol