反応 #2024505
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07855216B2
反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: tert-Butyl-dimethyl-chlorosilane (0.5 g, 3.21 mmol) was added to a stirred solution of isoxazolidin-4-ol hydrochloride (0.40 g, 3.18 mmol) in DMF (3 mL). The mixture was left to stir at ambient temperature for 2.5 hours before the solvent was evaporated and the resultant residue partitioned between ethyl acetate (50 mL) and water (20 mL). The organic phase was separated and washed with water (3×20 mL) then brine (20 mL), dried (MgSO4), filtered and evaporated to provide the desired product as a colourless oil (0.62 g, 96%). 1H NMR (CDCl3, 400 MHz) 5.52 (s, 1H), 4.60-4.65 (m, 1H), 3.45-3.62 (m, 1H), 3.80-4.05 (m, 1H), 2.80-3.05 (m, 2H), 0.80 (s, 9H), 0.08 (s, 6H). The mixture was left was evaporated the resultant residue partitioned between ethyl acetate (50 mL) and water (20 mL) The organic phase was separated washed with water (3×20 mL) brine (20 mL), dried (MgSO4) filtered evaporated
ソース ID: ord-ce8cdc3eb69547c19aff799da755fb5f