反応 #498441

反応方程式

2,3,5,6-tetrafluoro-4-[(2,2-dimethyldioxolan-4-yl)methoxy]pyridine

Cs2CO3

3-hydroxy-4-(benzyloxy)benzonitrile

→

3-[[3,5,6-trifluoro-4-[(2,2-dimethyldioxolan-4-yl)methoxy]pyridin-2-yl]oxy]4-(benzyloxy)benzonitrile

収率 56.1%

溶媒

CH3CN

反応条件

後処理

1. 1
   その他was partitioned with water and ethyl acetate
2. 2
   その他The layers were separated
3. 3
   洗浄washed with water and brine
4. 4
   乾燥dried (Na2SO4)
5. 5
   その他the solvent was removed in vacuo
6. 6
   その他The residue was triturated with hexane/ethyl acetate (1/1)
7. 7
   ろ過the resulting solid was collected by filtration

実験手順

To 2,3,5,6-tetrafluoro-4-[(2,2-dimethyldioxolan-4-yl)methoxy]pyridine (3.2 g, 11 mmol) in CH3CN (20 mL) was added Cs2CO3 (3.8 g, 12 mmol) and 3-hydroxy-4-(benzyloxy)benzonitrile (2.5 g, 11 mmol). After stirring for 24 hours the reaction was partitioned with water and ethyl acetate. The layers were separated, washed with water and brine, dried (Na2SO4), and the solvent was removed in vacuo. The residue was triturated with hexane/ethyl acetate (1/1) and the resulting solid was collected by filtration to give 3-[[3,5,6-trifluoro-4-[(2,2-dimethyldioxolan-4-yl)methoxy]pyridin-2-yl]oxy]4-(benzyloxy)benzonitrile (3.0 g).

出典