反应 #3758746
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08093427B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of fenbufen (214 mg, 0.8 mmol), HBTU (302 mg, 0.8 mmol), DIEA (1 mL, 0.8 mmol) and DMF (15 mL) was stirred. 4-azido-1-butanamine was added. TLC (acetone/n-hexane= 3/7) indicated the consumption of starting material (Rf=0.39) and the formation of the product (Rf=0.78). After stirring for 1 hr, the mixture was concentrated under high vacuum at 60° C. The residue was purified by flash chromatography using acetone: n-hexane=3:7 as eluents to provide a snow-white solid in 77% yield (269 mg). the consumption of starting material (Rf=0.39) the mixture was concentrated under high vacuum at 60° C The residue was purified by flash chromatography n-hexane=3:7 as eluents to provide a snow-white solid in 77% yield (269 mg)
来源 ID: ord-98b1634e93a64cb8be46531ac5ff23ad