反应详情

13 g of sodium azide and 59 ml of triethyl orthoformate are added to a solution of 13.4 g of 5-amino-valeric acid ethyl ester hydrochloride in 89 ml of acetic acid and the whole is stirred for 6 hours at 100°. The reaction mixture is cooled and partitioned betwen ethyl acetate and water. The organic phase is washed several times with saturated sodium bicarbonate solution and once with brine and, after drying over sodium sulphate, is concentrated. After purification by chromatography over silica gel (eluant: toluene/ethyl acetate 4:1 to 7:3), the pure title compound is obtained. Rf (toluene/ethyl acetate 1:1); 0.32.

1. temperatureThe reaction mixture is cooled
2. custompartitioned betwen ethyl acetate and water
3. washThe organic phase is washed several times with saturated sodium bicarbonate solution
4. dry with materialonce with brine and, after drying over sodium sulphate
5. concentrationis concentrated
6. customAfter purification by chromatography over silica gel (eluant: toluene/ethyl acetate 4:1 to 7:3)