反应详情

Lithium hydroxide monohydrate (0.30 g, 7.07 mmol) was added at room temperature to a solution of 300a) (1.0 g, 2.36 mmol) in THF/water (1:1, 40 mL). The reaction mixture was stirred at this temperature for 16 h and then concentrated. The residue was diluted with water (20 mL) and washed with ethyl acetate (2×30 mL). The aqueous phase was adjusted with sodium hydrogen sulfate to a pH value of 2. The precipitating solid was filtered off through a sintered funnel and residual water was removed by azeotropic distillation with toluene. Light brown solid. Yield: 0.75 g (75% of theory)

1. concentrationconcentrated
2. additionThe residue was diluted with water (20 mL)
3. washwashed with ethyl acetate (2×30 mL)
4. filtrationThe precipitating solid was filtered off through a sintered funnel
5. customresidual water was removed by azeotropic distillation with toluene