反应 #2908759
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06943159B1
反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 4-bromo-N-pivaloylaniline (1.56 g, 6 mmol) in dry THF (50 ml) at −78° C. was added t-BuLi (1.5 M in pentane, 13.3 ml, 20 mmol) and the yellow mixture was stirred for 1 h at −78° C. under N2. The reaction was quenched with B(OCH3)3 (1.7 ml, 15 mmol) and stirred for another 1 h at −78° C. The reaction mixture was then warmed to room temperature and hydrolysed with 0.5 M hydrochloric acid (50 ml) and extracted with EtOAc (3×80 ml), dried (Na2SO4) and concentrated to ca. 40 ml. n-Hexane (120 ml) was added slowly and the colorless crystalline product was filtered off and dried, yielding 1.26 g (95%). stirred for another 1 h at −78° C extracted with EtOAc (3×80 ml) dried (Na2SO4) concentrated to ca. 40 ml n-Hexane (120 ml) was added slowly the colorless crystalline product was filtered off dried yielding 1.26 g (95%)
来源 ID: ord-623e775ec87a48e0b74d0d731fc70272