反应详情

A solution of Intermediate 14b (593 mg, 3.45 mmol) and 4-piperidinemethanol (1.59 g, 13.8 mmol) in NMP (10 mL) was heated in the microwave at 170° C. for 3 h. The cooled mixture was applied to an SCX-2 cartridge (70 g), washing with methanol then eluting basic components with 0.4-2 M NH3 in MeOH. Product containing fractions were combined and concentrated in vacuo. The residue was purified by FCC, using 0-15% MeOH in EtOAc, to give the title compound as a brown gum (481 mg, 56%). LCMS (Method 3): Rt 2.12 min, m/z 251 [MH+].

1. washwashing with methanol
2. washthen eluting basic components with 0.4-2 M NH3 in MeOH
3. additionProduct containing fractions
4. concentrationconcentrated in vacuo
5. customThe residue was purified by FCC