反应详情

温度

0 °C

A mixture of 1.82 g of tert-butyl hydrazinecarboxylate and 2.4 ml of triethylamine in 50 ml of DCM is cooled to 0° C., a solution of 5.24 g of the compound obtained in stage A in 50 ml of DCM is added and the mixture is left stirring while allowing the temperature to rise to AT. The reaction mixture is washed with water, with a buffer solution at pH=2 and with a saturated NaHCO3 solution, the organic phase is dried over MgSO4 and the solvent is evaporated under vacuum. The residue is taken up in isopropyl ether, pentane is added and the precipitate formed is filtered off. 6.2 g of the expected compound are obtained.

1. waitthe mixture is left
2. washThe reaction mixture is washed with water, with a buffer solution at pH=2 and with a saturated NaHCO3 solution
3. dry with materialthe organic phase is dried over MgSO4
4. customthe solvent is evaporated under vacuum
5. additionpentane is added
6. customthe precipitate formed
7. filtrationis filtered off