反应 #1176375
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04002647
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 9.4 g. of p-toluenesulfonyl chloride are added with ice cooling to a solution of 6.5 g. of 4,6-dimethyl-2-heptanol in 50 ml. of anhydrous pyridine and the mixture is left for 24 hours at 5° C. Thereafter, the mixture is poured onto ice-water and extracted three times with diethyl ether. The extracts are washed successively with cold 2-N aqueous hydrochloric acid solution, water and twice with saturated sodium chloride solution, dried over sodium sulfate/potassium carbonate and evaporated at room temperature, finally at 0.05 mmHg. There is obtained 1,3,5-trimethylhexyl p-toluenesulfonate which exhibits a spot in the thin-layer chromatogram [Rf = 0.43; hexane/ethyl acetate (9:1 parts by volume)]. Thereafter, the mixture is poured onto ice-water extracted three times with diethyl ether The extracts are washed successively with cold 2-N aqueous hydrochloric acid solution, water and twice with saturated sodium chloride solution dried over sodium sulfate/potassium carbonate evaporated at room temperature, finally at 0.05 mmHg
来源 ID: ord-e53402205a8d4c9c82f401fc7ed7a4f9