反应详情

To a solution of 223 (1.67 mg, 8.2 mmol) in ethanol (30 ml) at 0° C. was added sodium borohydride (618 mg, 16.3 mmol). The reaction mixture was stirred at rt for 3 h. Water (50 ml) was added and the aqueous layer neutralised (2M HCl) and extracted with ethyl acetate (3×60 ml). The combined organic layers were washed with brine (30 ml), dried (MgSO4) and concentrated in vacuo to afford the title compound (1.34 mg, 80%) as a white solid. mp=170-173° C. 1H NMR (270 MHz; DMSO-d6) 1.04 (6H, s, 2×CH3), 2.42 (2H, s, CH2), 3.70 (3H, s, OCH3), 3.72 (2H, s, CH2), 6.43 (1H, s, CH), 6.54 (1H, s, CH), 8.60 (1H, brs, NH). LC/MS (ES+) tr=1.19 min, m/z 208.23 (M++H). HRMS (ES+) calcd. for C12H17NO2 (M++H) 208.1332, found 208.1322.

1. extractionextracted with ethyl acetate (3×60 ml)
2. washThe combined organic layers were washed with brine (30 ml)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo