反应详情

The product from Example 23A (560 mg, 1.700 mmol) as a solution in 7 M ammonia/methanol (20 mL) was added to solvent-washed Raney®-nickel (2800 mg, 47.7 mmol) in a 250 mL stainless steel pressure bottle and stirred at room temperature for 24 hours under hydrogen (30 pounds per square inch). The mixture was filtered through a nylon membrane and was concentrated. The residue was dissolved in methanol/dichloromethane (1:1), filtered and concentrated to give a solid which was slurried in methanol, filtered and dried to give the title compound. MS (DCI) m/z 288 (M+H)+.

1. filtrationThe mixture was filtered through a nylon membrane
2. concentrationwas concentrated
3. dissolutionThe residue was dissolved in methanol/dichloromethane (1:1)
4. filtrationfiltered
5. concentrationconcentrated
6. customto give a solid which
7. filtrationfiltered
8. customdried