反应详情

7.65 g (14.6 mmole) of the compound from Example 5 was hydrogenated in 80 ml of acetic acid at 70° C. and 50 psi pressure in a 250 ml Parr shaker using 5% palladium on carbon as the catalyst. Theoretical hydrogen uptake occurred at 40 minutes. The shaker was cooled and vented, and its contents filtered. The filtrate was placed in a rotary evaporator and the acetic acid was removed by azeotropation three times with toluene and then once with methyl alcohol. Recrystallization from ethyl acetatehexane yielded 6.7 g (89%) of the title compound, mp 57°-58°, Calc: C, 70.29; H, 7.86; Found C, 70.09; H, 7.76.

1. temperatureThe shaker was cooled
2. filtrationits contents filtered
3. customThe filtrate was placed in a rotary evaporator
4. customthe acetic acid was removed by azeotropation three times with toluene
5. customRecrystallization from ethyl acetatehexane