反应 #1520680
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09266892B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The reaction mixture of 4-bromo-2-methylphenol (Aldrich, Cat. No. 681121) (0.50 g, 2.7 mmol), 2-chloro-N,N-dimethylacetamide (Aldrich, Cat. No. 24350) (0.27 mL, 2.7 mmol) and potassium carbonate (1.1 g, 8.0 mmol) in DMF (4 mL) was stirred at 60° C. overnight. After cooling to r.t., the mixture was adjusted to pH˜2 with aqueous HCl, and extracted with ethyl acetate (3×20 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure to afford the product which was directly used in nest step reaction without further purification. LCMS (M+H)+=272.2/274.2. extracted with ethyl acetate (3×20 mL) The combined organic layers were dried over MgSO4 filtered concentrated under reduced pressure to afford the product which was directly used in nest step reaction without further purification
来源 ID: ord-00df84aad84b4400bbd10fce70253f37