反应详情

27.1 g (0.71 mol) of lithium aluminium hydride in 300 ml of absolute tetrahydrofuran are initially introduced into the reaction vessel, under nitrogen, and a solution of 57 g (0.21 mol) of 4-(tert.-butyloxycarbonylamino)-1,3-dioxo-1,3,3a,4,7,7a-hexahydroisoindole in 570 ml of absolute tetrahydrofuran is added dropwise. The mixture is then boiled under reflux cooling overnight. After cooling, 27.1 g of water in 82 ml of tetrahydrofuran, 27.1 g of 10% strength sodium hydroxide solution and 81.3 g of water are added dropwise to the batch in succession. The salts are filtered off with suction and washed with tetrahydrofuran and the filtrate is concentrated in vacuo. The residue is distilled under a high vacuum.

1. temperatureunder reflux
2. temperaturecooling overnight
3. temperatureAfter cooling
4. filtrationThe salts are filtered off with suction
5. washwashed with tetrahydrofuran
6. concentrationthe filtrate is concentrated in vacuo
7. distillationThe residue is distilled under a high vacuum