反应 #3731160
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06803378B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 4,4′-dichlorobenzhydryl chloride (3.22 g, 11.85 mmol) in a 1.85 M solution of methylamine in tetrahydrofuran (40 ml) was heated at 125° C. in a pressure vessel for 24 h. The cooled reaction mixture was diluted with ethyl acetate, washed with sodium carbonate, brine and dried (magnesium sulfate). Evaporation of the solvent and chromatography of the residue on silica gel (elution toluene-ethyl acetate 8:2) gave 2.12 g (67%) of the title amine as a clear oil. 1HNMR 400 MHz (CDCl3) δ (ppm): 2.57 (3H, s, NCH3), 4.85 (1H, s, CH benzhydryl), 7.0-7.53 (8H, m, aromatics). MS (ESI+) (m/z): 266 (M+H). The cooled reaction mixture washed with sodium carbonate, brine dried (magnesium sulfate) Evaporation of the solvent and chromatography of the residue on silica gel (elution toluene-ethyl acetate 8:2)
来源 ID: ord-6d37b2411615427c8fec0ebe4c06b3d7