反応 #1201535
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07622501B2
反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2.5 g of 2,3-bis(nitrooxy)propyl acetate in 25 mL of ethanol at 0. ° C. was added 469 mg of crushed NaOH powder. The reaction was stirred at 0° C. for 15 min upon which a cloudy suspension had formed. The resulting mixture was then poured onto ice cold 5% HCl and then extracted 3× with ether. The organics were combined and evaporated to remove most of the ethanol. The oil was then redissolved in ether, dried (Na2SO4), filtered and concentrated in vacuo to give a pale yellow oil which was used immediately without further purification. 1H NMR (500 MHz, acetone-d6): δ 5.59-5.52 (m, 1H), 5.05 (dd, 1H), 4.86 (dd, 1H), 4.60-4.50 (bs, OH), 3.95 (dd, 2H). had formed The resulting mixture was then poured onto ice cold 5% HCl extracted 3× with ether evaporated to remove most of the ethanol The oil was then redissolved in ether dried (Na2SO4) filtered concentrated in vacuo to give a pale yellow oil which was used immediately without further purification
ソース ID: ord-bc5a1a43b9e141f6aee726600c0c4b6c