反应详情

A solution of DMF (2.5 eq) and POCl3 (1.5 eq.) at 0° C. was stirred for 15 min. To that ethyl 4-oxopiperidine-1-carboxylate (1.0 eq) obtained from step I was added at 40° C. and reaction was continued at room temperature for 2 h Reaction was quenched with water and extracted with ethyl acetate, organic layer was separated, dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford crude product, which, on purification by column chromatography afforded the desired ethyl 4-chloro-5-formyl-3,6-dihydropyridine-1(2H)-carboxylate.

1. customreaction
2. customReaction
3. customwas quenched with water
4. extractionextracted with ethyl acetate, organic layer
5. customwas separated
6. dry with materialdried over anhydrous Na2SO4
7. concentrationconcentrated under reduced pressure
8. customto afford crude product, which
9. customon purification by column chromatography