反应详情

To a suspension of NaOtBu (4.23 g, 34.57 mM) in THF (50 mL) was added a mixture of ethyl 3-amino-1-benzyl-1,2,5,6-tetrahydropyridine-4-carboxylate (3.0 g, 11.52 mM) and methyl 3,3-dimethoxypropanoate (5.12 g, 34.57 mM) in THF (20 mL) in one portion and the mixture was agitated at ambient temperature overnight. The mixture was concentrated to half the volume before being quenched with ice-cold water. The homogeneous solution was extracted ethyl ether and the aqueous layer was carefully acidified with HCl until acidic. The precipitate was filtered, washed with water, and dried under vacuum to obtain the title compound as an off-white solid (1.6 g, 47%).

1. additionwas added
2. concentrationThe mixture was concentrated to half the volume
3. custombefore being quenched with ice-cold water
4. extractionThe homogeneous solution was extracted ethyl ether
5. filtrationThe precipitate was filtered
6. washwashed with water
7. customdried under vacuum