反应详情

The product from Example 11 (50.0 g; 178 mmol) is dissolved in anhydrous pyridine (910 ml). Methanesulphonyl chloride (18.6 ml; 241 mmol) is added dropwise while cooling in ice. Subsequently, the solution is stirred for 2.5 h during which it is allowed to warm to room temperature. The solution is then diluted with dichloromethane (3.6 l) and extracted twice by shaking with a 10% solution of sodium hydrogen carbonate (1.1 l on each occasion). The organic phase is dried (magnesium sulphate), concentrated and the residue subsequently distilled repeatedly with toluene. Yield: 64.0 g (quantitative).

1. temperaturewhile cooling in ice
2. extractionextracted twice
3. stirringby shaking with a 10% solution of sodium hydrogen carbonate (1.1 l on each occasion)
4. dry with materialThe organic phase is dried (magnesium sulphate)
5. concentrationconcentrated
6. distillationthe residue subsequently distilled repeatedly with toluene