反应详情

To a solution of 45.00 g (135.82 mmol) of (+/−)-6-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-5-oxo-[1,4]diazepane-1-carboxylic acid ethyl ester in 339 mL of anhydrous dichloromethane was added 22.09 g (149.40 mmol) of trimethyloxonium tetrafluoroborate. The resulting mixture was stirred at room temperature for 12 h. The mixture was hydrolyzed with a saturated aqueous solution of sodium hydrogen carbonate, extracted with dichloromethane, dried over sodium sulfate and the solvent was evaporated to afford 46.90 g (99%) of pure product as yellow oil. The compound was used as such in the next step.

1. extractionextracted with dichloromethane
2. dry with materialdried over sodium sulfate
3. customthe solvent was evaporated