反应详情

(+/−)-Trans-benzyl 3-methoxy-4-(tosyloxy)pyrrolidine-1-carboxylate (10.3 g, 25.4 mmol) was added to the soln. of sodium azide (5.78 g, 89 mmol) in water (10 mL) and DMF (60 mL) and heated to 100 deg. Celsius overnight. Diluted with EA/water and stirred. The organic layer dried (Na2SO4) and concentrated to give (+/−)-Cis-benzyl 3-azido-4-methoxypyrrolidine-1-carboxylate (6.3 g, 22.80 mmol, 90% yield). 1H NMR (400 MHz, chloroform-d) δ ppm 7.34-7.43 (5 H, m), 5.13-5.21 (2 H, m), 4.01-4.04 (2 H, m), 3.47 (3 H, s), 3.49-3.69 (4 H, m), Hz), LCMS: M+23=299, Rt=2.15 min.

1. dry with materialThe organic layer dried (Na2SO4)
2. concentrationconcentrated