反应详情

240 ml of a 1N sodium hydroxide solution are added to a suspension of 30.3 g (62 mmol) of diethyl[(tert-butoxycarbonyl)amino](3-iodobenzyl)malonate (Example 7D) in 440 ml of a mixture of ethanol and water (3:1). After 3 h under reflux and after cooling to RT, the pH of the reaction mixture is adjusted with concentrated hydrochloric acid to approx. pH 2. The reaction mixture is concentrated in vacuo. The residue is taken up in MTBE and water. The aqueous phase is extracted three times with MTBE. The combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue is purified by RP-HPLC (acetonitrile/water gradient).

1. temperatureAfter 3 h under reflux
2. concentrationThe reaction mixture is concentrated in vacuo
3. extractionThe aqueous phase is extracted three times with MTBE
4. dry with materialThe combined organic phases are dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue is purified by RP-HPLC (acetonitrile/water gradient)