反应 #2163016
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08268878B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 2-(4-chlorophenylthio)benzaldehyde (2.00 g, 8.00 mmol) in dichloromethane (20 mL) at 0° C. was added meta chloroperoxybenzoic acid (77% max, 5.40 g, 24.17 mmol) in, portions over 15 minutes, then warmed to room temperature and stirred for 2 hours. Aqueous sodium metabisulfite solution was added carefully until effervescence ceased. This solution was extracted with dichloromethane and the combined organic extracts were washed with NaOH (1N) then saturated brine, dried over MgSO4 and concentrated in vacuo giving a white solid (1.05 g, 3.74 mmol, 46%). δH (300 MHz, d6-DMSO) 10.69 (1H, s, CHO), 8.25-8.18 (1H, m, Ar), 8.07-8.00 (2H, m, Ar), 8.00-7.90 (3H, m, Ar) and 7.81-7.64 (3H, m, Ar). This solution was extracted with dichloromethane the combined organic extracts were washed with NaOH (1N) saturated brine, dried over MgSO4 concentrated in vacuo
来源 ID: ord-06f4df00109448608fae54363a4d7e2f