反应详情

To a solution of the product from step C (135 mg, 0.30 mmol) in dichloromethane (1 mL) and methanol (0.5 mL) was added 2M HCl in diethyl ether (4 mL). After stirring for 14 h at ambient temperature the reaction mixture was diluted with diethyl ether to induce precipitation. The reaction mixture was concentrated in vacuo to give 8-(3-fluorophenylsulfonyl)-1,2,3,4-tetrahydrobenzofuro[3,2-c]pyridine hydrochloride (96 mg, 96%, AUC HPLC>99%) as an off-white solid: mp 262-272° C. dec; 1H NMR (CD3OD, 300 MHz) δ 8.31-8.27 (m, 1H), 7.97 (dd, J=8.7, 2.1 Hz, 1H), 7.84-7.78 (m, 1H), 7.76-7.69 (m, 2H), 7.64-7.56 (m, 1H), 7.42-7.35 (m, 1H), 4.49 (s, 2H), 3.69 (t, J=6.0 Hz, 2H), 3.23-3.17 (m, 2H); APCI MS m/z 332 [M+H]+.

1. customprecipitation
2. concentrationThe reaction mixture was concentrated in vacuo