반응 #565199
ord-861a8f79424c42aaa0bb924f35a243a6
반응 방정식
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1추출extracted with 150 mL CHCl3 (3×50 mL)
- 2추출The CHCl3 extract
- 3건조was dried (MgSO4)
- 4기타evaporated
- 5기타The residue was recrystallized from THF-petroleum ether yielding 600 mg (47.4%), mp 270-71 C
- 6기타IR: (KBr): No C=O absorption at 1720 cm-1
실험 절차
A solution of oxymorphone (1.2 g, 4 mmol) and hydroxylamine hydrochloride (0.35 g, 5 mmol) in 20 mL of methanol was treated with 2 mL of 10% aqueous NaOH and stirred at room temperature for 15 h. The reaction mixture was poured into water and extracted with 150 mL CHCl3 (3×50 mL). The CHCl3 extract was dried (MgSO4), and evaporated. The residue was recrystallized from THF-petroleum ether yielding 600 mg (47.4%), mp 270-71 C. IR: (KBr): No C=O absorption at 1720 cm-1. 1H NMR (d6DMSO) δ 4.83 (s, C5H), Rf: silica gel EtOAc-EtOH-NH40H (100:1:1) 0.18. Anal. Calcd for C17H20N2O4 :C, 64.54; H, 6.37; N, 8.86. Found C, 64.76; H, 6.5; N, 8.58.