反应详情

温度

0 °C

To a cooled (0° C.) solution of 1-methoxy naphthalene (5 cm3, 34.5 mmol) in dichloromethane (20 cm3) was added, over a 10 minute period, chlorosulfonic acid (4.6 cm3, 69.0 mmol). Following this addition, phosphorus pentachloride (7.2 g, 34.5 mmol) was added and the reaction was maintained at 0° C. for a further 45 min. The reaction was then quenched by pouring onto ice/water (50 cm3), and allowed to warm to room temperature. Further dichloromethane (40 cm3) was added and the solution was transferred to a separating funnel, where the organic layer was collected and washed with saturated aqueous sodium chloride solution (70 cm3) and dried over sodium sulfate. The solvent was then evaporated under reduced pressure to afford title compound (8.23 g, 32.1 mmol; 93%).

1. additionwas added, over a 10 minute period
2. additionwas added
3. customThe reaction was then quenched
4. additionby pouring onto ice/water (50 cm3)
5. temperatureto warm to room temperature
6. additionFurther dichloromethane (40 cm3) was added
7. customthe solution was transferred to a separating funnel
8. customwhere the organic layer was collected
9. washwashed with saturated aqueous sodium chloride solution (70 cm3)
10. dry with materialdried over sodium sulfate
11. customThe solvent was then evaporated under reduced pressure