反应详情

温度

125 °C

Sodium azide (6.96 g, 0.107 mol) and ammonium chloride (2.13 g, 0.0399 mol) were added to a solution of 1-(tert-butoxy carbonyl)3-[(methylsulphonyl)oxy]piperidine (10 g, 0.0358 mol) in DMF (75 ml) and water (12.5 ml). The mixture was heated overnight at 125° C. under stirring, cooled and diluted with water and extracted with chloroform. The organic layer was washed with water, dried over Na2SO4 and concentrated to give 4.6 g of thin reddish brown oil. 1H NMR (CDCl3) δ: 2.80-4.30 (m, 5H), 1.60-2.20 (m, 4H), 1.50 (s, 9H).

1. temperaturecooled
2. extractionextracted with chloroform
3. washThe organic layer was washed with water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated