反应 #3745108
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08754076B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Hydrochloric acid (4 mol/L in 1,4-dioxane, 46 mL) was added to a solution of (R)-2-methyl-propane-2-sulfinic acid [(S)-1-(4-bromo-2-methyl-phenyl)-ethyl]amide (crude from Step 2, 8.85 g, ca. 75% pure) in ethyl acetate (80 mL) at room temperature. The solution was stirred at room temperature for 1 h and then concentrated. The residue was taken up in water and the resulting mixture was washed with diethyl ether. The aqueous phase was basified using aqueous 1 M NaOH solution and extracted with dichloromethane. The combined extracts were washed with brine, dried (MgSO4), and concentrated to afford the title compound. Yield: 4.04 g (905 of theory); Mass spectrum (ESI−): m/z=214/216 (Br) [m+H]+. concentrated the resulting mixture was washed with diethyl ether extracted with dichloromethane The combined extracts were washed with brine dried (MgSO4) concentrated
来源 ID: ord-66146b30c70a4d7db402106075e5307e