反应详情

To (S)-2-(6-methoxy-naphthalen-2-yl)-propan-ol (8.0 g, 37 mmol) in CH2Cl2 (200 mL) at 0° C. under N2 was added trichloroacetyl isocyanate (5.5 mL, 44 mmol). After the mixture was stirred at room temperature for 1 hr, the solvent was concentrated. The residue was treated MeOH (300 mL), water (40 mL) and potassium carbonate (21 g, 0.15 mol) and stirred at RT for 2 hrs to form white precipitate. The precipitate was collected by filtration and dissolved with CH2Cl2. The organic phase was washed with water, dried over MgSO4 and concentrated to give 5.5 g of white precipitate (57%).

1. concentrationthe solvent was concentrated
2. stirringstirred at RT for 2 hrs
3. customto form white precipitate
4. filtrationThe precipitate was collected by filtration
5. dissolutiondissolved with CH2Cl2
6. washThe organic phase was washed with water
7. dry with materialdried over MgSO4
8. concentrationconcentrated