反应 #1212931
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04179441
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A 20.2-g (0.2 mol) sample of triethylamine was added dropwise over 20 minutes to a stirred and cooled (ice bath) mixture of 9.3 g (0.1 mol) aminoacetonitrile hydrochloride in 150 ml chloroform. A solution of 13.2 g (0.1 mol) 2-furoyl chloride in 25 ml dichloromethane was then added dropwise over 20 minutes. The ice bath was removed and the reaction mixture stirred for 25 minutes. The reaction mixture was then washed with water, dried over magnesium sulfate and evaporated to give 7.4 g of crude N-cyanomethyl-2-furamide, as a beige solid, m.p. 85°-93° C. Recrystallization from benzene gave the furamide as a white solid, m.p. 101°-102° C. Elemental analysis for C7H6N2O showed: %C, calc. 56.0, found 56.0; %H, calc. 4.06, found 4.11; %N, calc. 18.7, found 19.1. cooled The ice bath was removed the reaction mixture stirred for 25 minutes The reaction mixture was then washed with water dried over magnesium sulfate evaporated
来源 ID: ord-d11b59c6d1124b568a5ad86dfe8389f5