تفاعل #1828902
ord-486a301b1a5548ff918bdedb400cea72
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1استخلاصThe resulting solution is extracted with EtOAc (2×400 ml)
- 2غسيلthe combined EtOAc portions washed with 2N HCl (800 ml), saturated NaCl solution (800 ml)
- 3تجفيفdried over MgSO4
- 4تركيزconcentrated in vacuo
- 5أخرىThe resulting solid is recrystallized from EtOAc/hexanes
الإجراء التجريبي
To a solution of 2-(4'-fluoro-4-biphenylylmethyl)-6-[2-(N-hydroxyamino)ethoxy]-1-oxo-1,2,3,4-tetrahydroisoquinoline (~22.5 mmol) in 1,4-dioxane (50 ml) and methylene chloride (30 ml), is added trimethylsilylisocyanate (3.36 ml). The reaction mixture is stirred at room temperature overnight and is subsequently diluted with H2O (500 ml). The resulting solution is extracted with EtOAc (2×400 ml) and the combined EtOAc portions washed with 2N HCl (800 ml), saturated NaCl solution (800 ml), dried over MgSO4, and concentrated in vacuo. The resulting solid is recrystallized from EtOAc/hexanes to give 2-(4'-fluoro-4-biphenylylmethyl)-6-[2-(N-aminocarbonyl-N-hydroxyamino)-ethoxy]-1-oxo-1,2,3,4-tetrahydroisoquinoline, m.p. 171°-172°.