反应 #1626147
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06534447B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1A (0.55 g), 2-(trifluoromethylthio)-ethanol (0.35 g, Example A), triphenylphosphine (0.64 g) and diethyl azodicarboxylate (0.42 g) in dry tetrahydrofuran (5 ml) is stirred for 20 hours at ambient temperature. The reaction mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields 0.45 g of the title compound as an colorless oil. filtered through a bed of silica gel The filtrate is washed with water The organic layer is dried with anhydrous magnesium sulfate filtered evaporated in vacuo Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)
来源 ID: ord-fad1989119e94b57b3eb3c7f9657511f