反应 #1263309
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09198845B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: At 5° C., a suspension of L-(+)-glutamine (23.1 g, 158 mmol) in 1:1 water/dioxane (300 ml) was treated successively with a solution of 2N aq. NaOH (79 ml) and with 2-ethylhexyl isocyanate (25 g, 158 mmol). The resulting mixture was stirred for 24 h while its temperature rose to 20° C. (final pH value: 6) and filtered. The filtrate was washed twice with ethyl acetate (200 ml) and the combined organic phases were acidify with a 2N aq. HCl solution to pH 1. Filtration of the resulting precipitate and drying under vacuum gave N2-[(2-ethylhexylamino)carbonyl]-L-glutamine (42 g, 88%, white solid). rose to 20° C. filtered The filtrate was washed twice with ethyl acetate (200 ml) Filtration of the resulting precipitate drying under vacuum
来源 ID: ord-bddc4e1bf68b4a66a509a3f02032a1ab