反应 #2008384
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05241076
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 115 g (0.65 mol) of ethyl N-(2,2-dimethoxyethyl)-carbamate, 130 g of powdered potassium hydroxide and 2 g of triethylbenzylammonium chloride are initially introduced into 650 ml of toluene and 142 g (0.7 mol) of 2chloroallyl iodide are added dropwise at room temperature. After stirring overnight, a gas chromatogram showed incomplete conversion, hence 65 g of powdered potassium hydroxide and 1 g of triethylbenzylammonium chloride were added again and a further 71 g (0.35 mol) of 2-chloroallyl iodide were added dropwise. After stirring overnight at room temperature, the salts were filtered off with suction, the filtrate was washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated, and the residue was distilled. are added dropwise at room temperature were added again After stirring overnight at room temperature the salts were filtered off with suction the filtrate was washed with saturated sodium chloride solution dried over magnesium sulphate concentrated the residue was distilled
来源 ID: ord-e292966163114a43989588e032b9a884