反应详情

To a solution of the methyl ester of Example 32j (0.280 g, 0.7 mmols) in DMF (10 mL) was added activated Raney-Nickel (100 mg) and the reaction mixture was subjected to reduction in a Parr hydrogenator (20 psi, 2 h). The reaction mixture was filtered (celite bed), and the filtrate was poured onto crushed ice to obtain a solid which was subjected to hydrolysis as described in the synthesis of Example 11 to obtain the title compound. Yield: 76%; 1H NMR (DMSO-d6): δ 2.60 (s, 3H, CH3), 5.10 (s, 2H, CH2), 5.40 (s, 2H, NH2), 6.80 (d, 2H, Ar), 8.10 (s, 1H, Ar), 8.20 (s, 1H, Ar); MS: m/e (EI+) 354 (M+1).

1. customwas subjected to reduction in a Parr hydrogenator (20 psi, 2 h)
2. filtrationThe reaction mixture was filtered (celite bed)
3. additionthe filtrate was poured
4. customonto crushed ice
5. customto obtain a solid which
6. customwas subjected to hydrolysis
7. customas described in the synthesis of Example 11