反应详情

温度

20 °C

2.8 cm3 (20 mmol) of triethylamine and 3.2 g (20 mmol) of 3-cyanophenyl isothiocyanate are added at 0° C. to a solution of 3.35 g (20 mmol) of glycine t-butyl ester in 150 cm3 of dichloromethane. The mixture is stirred at 20° C. for 12 hours before being concentrated under vacuum and then taken up with a mixture of water and ethyl ether (300:300). The ether phase is separated off and washed with a 1N hydrogen chloride solution (200 cm3), and then with a saturated sodium chloride solution. After drying with magnesium sulfate and concentration under vacuum, 5.17 g (89% yield) of a yellow solid is obtained, whose melting point is 131°-132° C.

1. concentrationbefore being concentrated under vacuum
2. additiontaken up with a mixture of water and ethyl ether (300:300)
3. customThe ether phase is separated off
4. washwashed with a 1N hydrogen chloride solution (200 cm3)
5. dry with materialAfter drying with magnesium sulfate and concentration under vacuum