反应详情

温度

50 °C

To a stirred solution of 3-azido-3-methylbutanoic acid (10 g, 69.8 mmol) in anh. dichloroethane (50 mL) was added thionyl chloride in one portion (10.0 mL, 2 equiv, 0.14 mol). The flask was fitted with a condenser and the reaction was heated in a 50° C. oil bath for 2 h. The reaction was concentrated to a brown-black suspension. The residue was vacuum distilled through a short path distillation apparatus. The forerun was discarded and the major fraction distilled at 66° C. at 18 mbar as a pale yellow liquid (9.66 g, 85.6%). 1H NMR (CDCl3, 400 MHz): δ 1.41 (s, 6H), 2.51 (s, 2H), 2.98 (s, 2 H).

1. customThe flask was fitted with a condenser
2. concentrationThe reaction was concentrated to a brown-black suspension
3. distillationdistilled through a short path distillation apparatus
4. distillationthe major fraction distilled at 66° C. at 18 mbar as a pale yellow liquid (9.66 g, 85.6%)