反应详情

Add LiHMDS (1M in THF, 21.38 mL, 21.38 mmol) to (methoxymethyl)triphenyl-phosphonium chloride (7.329 g, 21.38 mmol) in THF (51.0 mL) via syringe at 0° C. and stir. After 30 minutes, add (S)-(1,4-dibenzyl-piperazin-2-yl)-acetaldehyde (4.71 g, 15.27 mmol) in THF (51.0 mL) via syringe. Remove ice bath and stir at ambient temperature. After 4 hours, add water and extract with ethyl acetate twice. Combine the organic solution, dry over sodium sulfate, filter, and concentrate under reduced pressure to give crude residue. Purify the residue by flash chromatography, eluting with ethyl acetate:hexane (40:60) to give the title compound: mass spectrum (m/e):337.18 (M+1).

1. stirringRemove ice bath and stir at ambient temperature
2. waitAfter 4 hours
3. extractionextract with ethyl acetate twice
4. dry with materialdry over sodium sulfate
5. filtrationfilter
6. concentrationconcentrate under reduced pressure
7. customto give crude residue
8. customPurify the residue by flash chromatography
9. washeluting with ethyl acetate:hexane (40:60)