反応 #644441

反応方程式

sodium hydride

1,4-benzenedimethanol

2-fluoropyridine

N,N-dimethyl formamide

→

title compound

収率 67.9%

(4-(Pyridin-2-yloxymethyl)-phenyl)methanol

収率 67.9%

溶媒

water

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with saturated sodium chloride water
3. 3
   その他the solvent thereof was evaporated under a reduced pressure
4. 4
   その他The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1)

実験手順

To a mixture of 1,4-benzenedimethanol (5.5 g, 40 mmol), 2-fluoropyridine (1.3 g, 13 mmol), and N,N-dimethyl formamide (15 mL) was added sodium hydride (1.4 g, 40 mmol, 66% in oil) at 0° C, which was stirred at room temperature for 20 minutes and at 70° C for one hour. To the reaction mixture was added water, and extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride water, and the solvent thereof was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1) to obtain the title compound (1.9 g).

出典