反应详情

The product from Example 1 (10.0 g; 38 mmol) is dissolved in anhydrous pyridine (185 ml), and methanesulphonyl chloride (3.7 ml; 46 mmol) is slowly added dropwise at 0° C. The solution is stirred at room temperature for 6.5 h. Subsequently, the solution is diluted with dichloromethane (740 ml) and extracted twice with a 10% solution of sodium hydrogen carbonate (250 ml on each occasion). The organic phase is dried (magnesium sulphate) and concentrated, and the residue is subsequently distilled repeatedly with toluene. Yield: 10.79 g (85%), brown oil.

1. extractionextracted twice with a 10% solution of sodium hydrogen carbonate (250 ml on each occasion)
2. dry with materialThe organic phase is dried (magnesium sulphate)
3. concentrationconcentrated
4. distillationthe residue is subsequently distilled repeatedly with toluene