反应详情

温度

-78 °C

To reactant 155a (4.8 g, 19.8 mmol) suspended in anhydrous THF (100 mL) at −78° C., was added 2.0 M LDA in Hexane (14.9 mL, 29.7 mmol) over 20 min period. The mixture was stirred at −78° C. for 45 min, then let it warm up to 0° C. over 3 hour. Reaction was monitored by TLC. After completion, the reaction was quenched by adding aq. 10% citric acid slowly. It was extracted with EtOAc twice, washed with brine. The organic layer was dried through (Na2SO4), and concentrated; the residue was purified by CombiFlash using EtOAC/Hexane as eluents to give (3S,7aS)-1-oxo-3-(trichloromethyl)hexahydropyrrolo-[1,2-c]oxazole-7a-carbaldehyde 155b 1.99 g, 37%.

1. temperaturewarm up to 0° C. over 3 hour
2. customReaction
3. customAfter completion, the reaction was quenched
4. additionby adding aq. 10% citric acid slowly
5. extractionIt was extracted with EtOAc twice
6. washwashed with brine
7. dry with materialThe organic layer was dried through (Na2SO4)
8. concentrationconcentrated
9. customthe residue was purified by CombiFlash