反応 #161511

反応方程式

Cycloheptylmethanol

3-bromophenol

→

((3-bromophenoxy)methyl)cycloheptane

反応条件

後処理

1. 1
   濃縮After concentration under reduced pressure, hexanes
2. 2
   workup.ADDITIONwas added
3. 3
   その他sonicated
4. 4
   その他the precipitate was removed by filtration
5. 5
   洗浄the solids washed with hexanes
6. 6
   濃縮The combined filtrates were concentrated under reduced pressure
7. 7
   その他Purification by flash chromatography (10 to 50% EtOAc-hexanes gradient)

実験手順

Cycloheptylmethanol was coupled with 3-bromophenol following the method used in Example 10. After concentration under reduced pressure, hexanes was added. The mixture was stirred and sonicated then the precipitate was removed by filtration and the solids washed with hexanes. The combined filtrates were concentrated under reduced pressure. Purification by flash chromatography (10 to 50% EtOAc-hexanes gradient) gave ((3-bromophenoxy)methyl)cycloheptane. (Yield 1.0697 g, 56%): 1H NMR (400 MHz, CDCl3) δ 7.12 (t, J=8.4, 1H), 7.06-7.04 (m, 2H), 6.82 (dq, J=8.0, 1.2, 1H), 3.70 (d, J=6.4, 2H), 1.91-1.98 (m, 1H), 1.81-1.88 (m, 2H), 1.42-1.72 (m, 8H), 1.24-1.34 (m, 2H).

出典