反应详情

A solution of the product from Example 83 (1 g, 2.7 mmol) in 250 mL acetic acid was treated with 20% Pd/C (0.1 g) and shaken on a Parr apparatus under 52 psi hydrogen gas for 21 hours. After removal of the catalyst, the solvent was evaporated but gave negligible material. The catalyst/celite was washed two times with 1 N HCl, and the aqueous solution was basified with sodium bicarbonate. The precipitate was collected by filtration, dried and then recrystallized from methanol/dimethylformamide to give the title compound (0.26 g, 44% yield) mp>300° C.

1. customAfter removal of the catalyst
2. customthe solvent was evaporated
3. customgave negligible material
4. washThe catalyst/celite was washed two times with 1 N HCl
5. filtrationThe precipitate was collected by filtration
6. customdried
7. customrecrystallized from methanol/dimethylformamide