反应详情

温度

50 °C

To a stirred solution of N-hydroxyphthalimide (10.0 g, 61.30 mmol) in DMF (40 mL) at RT was added NEt3 (9.40 mL, 67.43 mmol) and, in a dropwise fashion, (bromomethyl)cyclohexane (9.41 mL, 67.43 mmol). The reaction was then stirred for 15 hours at 50° C., after which it was allowed to cool to RT and then concentrated under vacuum. The residue was dissolved in Et2O (100 mL) and washed with water, brine, dried over MgSO4 and the solvent removed under reduced pressure. The residue was purified by column chromatography (eluting with CH2Cl2/PE, 1:1 to 3:1) to afford N-(cyclohexylmethoxy)phthalimide (8.40 g, 53%), as a white solid.

1. temperatureto cool to RT
2. concentrationconcentrated under vacuum
3. dissolutionThe residue was dissolved in Et2O (100 mL)
4. washwashed with water, brine
5. dry with materialdried over MgSO4
6. customthe solvent removed under reduced pressure
7. customThe residue was purified by column chromatography (eluting with CH2Cl2/PE, 1:1 to 3:1)