反应详情

11.58 g of phenyl 3-amino-3-methylbutane-1-sulfonate and 5.34 g of KOH were boiled under reflux in 240 ml of THF/95 ml of water for 7 hours. Then a further 2.7 g of KOH, 50 ml of water and 120 ml of THF were added, and the mixture was again boiled under reflux for 7 hour. Then a further 5.34 g of KOH were added, and the mixture was again boiled under reflux for 3 hours. It was allowed to cool and then 300 ml of a 2N aqueous HCl solution were added, and the mixture was extracted 5 times with 250 ml of EA each time. After drying over Na2SO4, the solvent was removed in vacuo. Chromatography on silica gel with EA/HEP 1:1 afforded 3.82 g of white crystals, mp 72° C.

1. temperatureunder reflux for 7 hour
2. temperatureunder reflux for 3 hours
3. temperatureto cool
4. extractionthe mixture was extracted 5 times with 250 ml of EA each time
5. dry with materialAfter drying over Na2SO4
6. customthe solvent was removed in vacuo