反応 #3312149
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07265108B2
反応条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: After dissolving 8.17 g of 2-amino-3-(tert-butoxy)propionamide in 150 ml of dichloromethane, 16.37 ml of triethylamine was added and the solution was cooled to −78° C., and then 4.10 ml of thionyl chloride was added dropwise while stirring at below −50° C. After stirring for 30 minutes, the temperature was raised to room temperature and stirring was continued overnight. Water was added to the reaction solution, and extraction was performed with dichloromethane. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and filtered with silica gel. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain the title compound (1.98 g, 21% yield). was added After stirring for 30 minutes the temperature was raised to room temperature stirring The organic layer was washed with saturated brine dried over anhydrous magnesium sulfate filtered with silica gel The solvent was distilled off under reduced pressure the residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate)
ソース ID: ord-e239c92e238e49d39b27cd4e8a8585ea