反应 #2206591
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06815459B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 500 mg (2.0 mmol) of 2-bromo-3-nitrobenzoic acid in anhydrous THF (15 mL) was added 2.80 mL (4.47 mmol) of n-BuLi (1.6 M soln. in Hex.) slowly at −78° C. After 10 minutes, a solution of 383 mg (2.03 mmol) of dimethyl diselenide in THF (5 mL) was added. After 30 minutes, the reaction mixture was warmed to room temperature. After additional stirring for 2 hours, ethyl acetate was added. The organic layer was washed with 1 N HCl solution, dried over MgSO4, and concentrated under reduced pressure. 470 mg of crude product was obtained and used for the next reaction without further purification. After 30 minutes The organic layer was washed with 1 N HCl solution dried over MgSO4 concentrated under reduced pressure
来源 ID: ord-b026afd0448946b8bd3d04a092fda704