反应详情

温度

100 °C

A mixture of intermediate 59 (1.0 g, 0.0027 mol), 4-fluorobenzylamine (0.372 mL, 0.00321 mol) and MeOH (0.4 mL) is heated at 100° C. for 2 days. The reaction mixture is cooled to RT, and partitioned between dichloromethane and water. The organic solution is separated, dried (MgSO4), and concentrated in vacuo. The residue is purified by chromatography on silica gel; gradient elution with heptane:EtOAc (80:20-40:60) gives 0.50 g of the product 85. 1H NMR (CDCl3) δ 7.60-7.35 (m, 3H), 7.15-6.90 (m, 10H), 6.85-6.70 (m, 2H), 5.50-5.30 (m, 2H), 5.75-5.55 (m, 2H), 1.12 (s, 9H); MS: m/z 446 (M++1).

1. temperatureThe reaction mixture is cooled to RT
2. custompartitioned between dichloromethane and water
3. customThe organic solution is separated
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue is purified by chromatography on silica gel
7. washgradient elution with heptane:EtOAc (80:20-40:60)