反应详情

A solution of trifluoroacetic acid (18.8 mmol, 2.13 mL) and 2-Acetyl-3-methyl-8-(tert-butyloxycarbonyl)-8-azabicyclo [3.2.1]oct-2-en (0.49 g, 1.88 mmol) was stirred at room temperature for about 0.5 hour. The solution was concentrated three times under reduced pressure after the addition of hexane to remove excess trifluoroacetic acid. A concentrated solution of sodium carbonate was added to the residue to form a basic solution. The solution was extracted with methylene chloride, dried using sodium sulfate and purified by bulb-to-bulb distillation (80° C. (1.0 mmHg)) to give 2-acetyl-3-methyl-8-azabicyclo [3.2.1]oct-2-ene.

1. concentrationThe solution was concentrated three times under reduced pressure
2. additionafter the addition of hexane
3. customto remove excess trifluoroacetic acid
4. additionA concentrated solution of sodium carbonate was added to the residue
5. customto form a basic solution
6. extractionThe solution was extracted with methylene chloride
7. customdried
8. distillationpurified by bulb-to-bulb distillation (80° C. (1.0 mmHg))