反应详情

A solution of trifluoroacetic acid (18.8 mmol, 2.14 ml) and 2-acetyl-3-methyl-8-(tert-butoxycarbonyl)-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 under reduced pressure. Hexane was added to the resulting residue, the resulting solution was concentrated under reduced pressure, and the process was repeated a second time to remove any residual 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 under reduced pressure
2. additionHexane was added to the resulting residue
3. concentrationthe resulting solution was concentrated under reduced pressure
4. customto remove any residual trifluoroacetic acid
5. additionA concentrated solution of sodium carbonate was added to the residue
6. customto form a basic solution
7. extractionThe solution was extracted with methylene chloride
8. customdried
9. distillationpurified by bulb-to-bulb distillation (80° C. (1.0 mmHg))