反应详情

温度

45 °C

A mixture of tert-butyl 3-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)pyrazolo[1,5-a]pyrimidin-5-yl)-8-azabicyclo[3.2.1]oct-3-ene-8-carboxylate (12.2 g, 20.3 mmol) and 10% Pd/C (2.1 g) in EtOAc (175 ml) was stirred at 45° C. under hydrogen (balloon pressure) for 16 hours. After filtration and concentration, the crude mixture of two isomers was purified by gradient column chromatography on silica eluting with EtOAc/Hexanes (0-35%) to give the slightly impure “endo” product (6.24 g, Rf=0.6 in 25% EtOAc/Hexanes) and the “exo” product (5.44 g, Rf=0.5 in 25% EtOAc/Hexanes) which was used in the following reaction sequences.

1. filtrationAfter filtration and concentration
2. additionthe crude mixture of two isomers
3. customwas purified by gradient column chromatography on silica eluting with EtOAc/Hexanes (0-35%)
4. customto give the slightly impure “