反应详情

温度

80 °C

To a mixture of N,N-dimethylaminoethanol (4.16 g, 46.7 mmol) and (3-benzyloxy)-2-bromopyridine (from Step 1; 8.22 g, 31.1 mmol) in dry DMF (50 mL) was sodium tert-butoxide (5.98 g, 62.2 mmol) added in one portion. The reaction mixture was stirred at 80° C. for 1.5 h, the solvent was removed under reduced pressure and the oily residue was taken up between CHCl3/water. The aqueous phase was extracted twice with CHCl3 and the combined organic layers were washed once with brine, dried (MgSO4), and concentrated under reduced pressure. This gave 8.4 g (100%) of the title compound as a light brown oil. Purity 95% (HPLC). HRMS m/z calcd for C16H20N2O2 (M)+ 272.1525. found 272.1537.

1. additionadded in one portion
2. customthe solvent was removed under reduced pressure
3. extractionThe aqueous phase was extracted twice with CHCl3
4. washthe combined organic layers were washed once with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated under reduced pressure