反应详情

Stir a mixture of 1-(6-methylpyridin-3-yl)-ethanone (10 g, 74 mmol) in titanium tetra(isopropoxide) (42.1 g, 148 mmol) and ammonia (370 mmol, 2 M in methanol) under N2 for 6 h at RT. To this mixture add sodium tetrahydroborate (4.2 g, 111 mmol) and stir overnight. Quench the reaction mixture with ammonium hydroxide and filter the mixture. From the filtrate, remove the solvent and extract the residue with DCM, wash with saturated aqueous sodium chloride and dry over Na2SO4, filter, and remove the solvent to obtain the title compound as a dark yellow oil (8.16 g). MS (ES) m/z 137 [M+1]+.

1. stirringstir overnight
2. customQuench the reaction mixture with ammonium hydroxide
3. filtrationfilter the mixture
4. customFrom the filtrate, remove the solvent
5. extractionextract the residue with DCM
6. washwash with saturated aqueous sodium chloride
7. dry with materialdry over Na2SO4
8. filtrationfilter
9. customremove the solvent