反应详情

温度

100 °C

To a mixture of N-[4-(1,3,3-trimethyl-6-aza-bicyclo[3.2.1]octane-6-carbonyl)-phenyl]-acrylamide (0.2 g, 0.613 mmol) and piperidine (120 μl, 1.23 mmol) in EtOH (10 ml) was added two drops of TEA. The resulting mixture was heated in a microwave oven at 100° C. for 25 min. The volatiles were evaporated in vacuo and the residue purified on column chromatography (silicagel) using first EtOAc followed by 4% TEA in EtOAc-EtOH 9:1 as eluents. Semi pure fractions were collected, the solvent evaporated in vacuo and the residue dissolved in 1 N HCl (2.5 ml). Water (5 ml) was added followed by diethyl ether (10 ml) and the mixture was stirred for 30 min. The organic phase was discarded and the pH of the aqueous phase adjusted to 10 with 1 N NaOH followed by extraction with diethyl ether (2×10 ml). The combined organic phases were dried (Na2SO4), filtered and evaporated in vacuo affording 55 mg (22%) of the title compound as an oil.

1. customThe volatiles were evaporated in vacuo
2. customthe residue purified on column chromatography (silicagel)
3. customSemi pure fractions were collected
4. customthe solvent evaporated in vacuo
5. dissolutionthe residue dissolved in 1 N HCl (2.5 ml)
6. additionWater (5 ml) was added
7. extractionfollowed by extraction with diethyl ether (2×10 ml)
8. dry with materialThe combined organic phases were dried (Na2SO4)
9. filtrationfiltered
10. customevaporated in vacuo