反应详情

To a solution of ethyl glycolate (1 eq) in THF was added sodium hydride (2.5 eq) at 0° C. and the reaction mixture was stirred for 1 h 4-chloro-1-[(4-methylphenyl)sulfonyl]-1,2,5,6-tetrahydropyridine-3-carbaldehyde (1 eq) obtained in step II of example 200 in THF was added at 0° C. and was refluxed 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 ethyl 5-[(4-methylphenyl)sulfonyl]-4,5,6,7-tetrahydrofuro[3,2-c]pyridine-2-carboxylate.

1. additionwas added at 0° C.
2. temperaturewas refluxed for 2 h
3. customReaction
4. customwas quenched with water
5. extractionextracted with ethyl acetate, organic layer
6. customwas separated
7. dry with materialdried over anhydrous Na2SO4
8. concentrationconcentrated under reduced pressure
9. customto afford crude product, which
10. customon purification by column chromatography