反应 #1304780
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05090993
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A suspension of ethyl 2-(chlorosulfonyl)-3-nitrobenzoate (14.7 g), amino-t-butyldimethylsilane (15.4 g), and sodium bicarbonate (3.5 g) in dichloromethane (300 mL) was stirred at room temperature in a stoppered flask for 4 days. Water (90 mL) and saturated aqueous bicarbonate (45 mL) were added, and the mixture was stirred. The dichloromethane phase was dried over magnesium sulfate, filtered, concentrated, and chromatographed on silica gel eluted with 20% ethyl acetate in hexanes to give 12.9 g of the title compound as a white solid, m.p. 101-102° C. the mixture was stirred The dichloromethane phase was dried over magnesium sulfate filtered concentrated chromatographed on silica gel eluted with 20% ethyl acetate in hexanes
来源 ID: ord-d988b4de0dde46d5ba9741f8224bd56d