反应详情

Lithium hydroxide monohydrate (33 mg, 0.786 mmol) was added to an ice-cooled suspension of 331d) (0.22 g, 0.524 mmol) in THF/water (1:1, 10 mL) and the resulting mixture was stirred at room temperature for 48 h. The THF was distilled off and the residue was diluted with water (5 mL) and acidified with saturated sodium hydrogen sulfate solution. A precipitating solid was filtered off and washed with water. Remaining humidity was removed by repeated azeotropic distillation of toluene. White solid. Yield: 0.17 g (80% of theory)

1. temperaturecooled
2. distillationThe THF was distilled off
3. additionthe residue was diluted with water (5 mL)
4. filtrationA precipitating solid was filtered off
5. washwashed with water
6. customwas removed
7. distillationdistillation of toluene