反应详情

To a solution of 2-(bromomethyl)-4,6-dichlorobenzonitrile (1.3 mmol) (A.2.5.1) and 2-hydroxyethyl acetate (1.43 mmol) in 7 mL THF was added NaH (1.95 mmol, 60% suspension in oil). The reaction mixture was stirred at RT overnight and then poured into a 1M HCl solution. The mixture was extracted twice with EtOAc. The combined organic layers were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification with CC (KP-SIL™ from Biotage) using Hept to Hept/EtOAc (75/25) gives the desired compound as orange oil.

1. extractionThe mixture was extracted twice with EtOAc
2. washThe combined organic layers were washed with brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo
5. customPurification with CC (KP-SIL™ from Biotage)