反应详情

The product of Example 1 (0.81 g, 1.42 mmol) in MeOH (30 g) was dissolved in MeOH (8 mL) and 48% aqueous HBr solution (0.16 mL, 1.4 mmol) added. The mixture was stirred at rt for 1 hr and concentrated in vacuo. MeOH (1.6 mL) and MTBE (6.4 mL) was added to residue and the suspension stirred at rt for 4 days. The suspension was filtered, the collected solid washed with MTBE (50 mL) and dried to give the title compound (734 mg); MS multimode (+) 568; 1H NMR (DMSO-d6): δ 9.86 (brs, 1H), 7.24 (d, 2H), 7.18 (d, 2H), 6.42 (br, 2H), 4.12 (t, 2H), 3.69 (t, 4H), 3.65 (s, 3H), 3.50 (s, 2H), 3.08-2.97 (m, 6H), 2.41 (m, 4H), 1.83-1.51 (m, 12H), 1.40-1.32 (m, 2H), 0.90 (t, 3H).

1. concentrationconcentrated in vacuo
2. additionMeOH (1.6 mL) and MTBE (6.4 mL) was added to residue
3. stirringthe suspension stirred at rt for 4 days
4. filtrationThe suspension was filtered
5. washthe collected solid washed with MTBE (50 mL)
6. customdried