反应详情

To a solution of (S)-N-benzyl-1-phenylethanamine (3.64 g, 17.26 mmol) in THF (40 mL) at −70° C., was added dropwise n-BuLi (1.6 M, 14.7 mmol) over a period of 30 min and stirred further. After 1 h, a solution of (E)-tert-butyl 3-(6-methylpyridin-3-yl)acrylate (2.7 g, 12.3 mmol) in THF was added slowly to the above mixture and stirred further. After 2 h, sat. NH4Cl solution was added to the reaction mixture and extracted with EtOAc (3×). The combined organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo to afford a residue. Purification of the residue by column chromatography (Neutral Al2O3, Et2O/Pet ether 5:95) afforded the title compound. MS: 431.6 [M+H]+;

1. stirringstirred further
2. waitAfter 2 h
3. extractionextracted with EtOAc (3×)
4. dry with materialThe combined organic phase was dried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customto afford a residue
7. customPurification of the residue by column chromatography (Neutral Al2O3, Et2O/Pet ether 5:95)