反应详情

2-Indanol (20.00 g, 149.5 mmol) and diisopropylethylamine (21.2 g, 164 mmol) was stirred in dichloromethane (300 mL) at 0° C. Methanesulfonyl chloride (18.78 g, 164 mmol) and dimethylaminopyridine (1.80 g) were added simultaneously and stirring continued at room temperature for 18 h. Solution was evaporated, partitioned between ethyl acetate and water, and the organic phase separated. This was washed with NaHCO3 (sat) and with citric acid solution (5%) and dried over MgSO4. The filtered solution was concentrated and the resultant solid recrystallized from isopropanol-EtOH (3:1) to give off-white crystals (24.6 g, 78%).

1. customSolution was evaporated
2. custompartitioned between ethyl acetate and water
3. customthe organic phase separated
4. washThis was washed with NaHCO3 (sat) and with citric acid solution (5%)
5. dry with materialdried over MgSO4
6. concentrationThe filtered solution was concentrated
7. customthe resultant solid recrystallized from isopropanol-EtOH (3:1)