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HRID 52943作成日:2026年10月26日

Methylamine → N-methyl-1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-4-hydroxymethylimidazole-5-carboxamide

https://huagongshe.com/reaction/52943

反応式

関与物質

役割名称HCID仕込み量
反応物MethylamineHCID 6329—
反応物Succinimido 1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-4-hydroxymethylimidazole-5-carboxylateHCID 19036239—
溶媒MethanolHCID 887—
溶媒WaterHCID 962—
溶媒DichloromethaneHCID 6344—
生成物N-methyl-1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-4-hydroxymethylimidazole-5-carboxamideHCID 19036316—

反応手順

0.4 ml of a 40% by volume solution of methylamine in water was added at room temperature to a solution of 0.278 g of succinimido 1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-4-hydroxymethylimidazole-5-carboxylate [prepared as described in Example 52(a)] in a mixture of 3 ml of methylene chloride and 2 ml of methanol, and the resulting mixture was allowed to stand for 16 hours at room temperature. At the end of this time, the solution was concentrated by evaporation under reduced pressure, and the concentrate was dissolved in ethyl acetate. The resulting solution was washed with an aqueous solution of potassium bisulfate and with an aqueous solution of sodium hydrogencarbonate, in that order, after which it was dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, and the resulting residue was purified by column chromatography through silica gel, using ethyl acetate as the eluent, to give 176 mg of the title compound as a glass.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05616599
出典データセットuspto-grants-1997_04
ORD IDord-7c2def88fa374aaaa43921cb4adb7f74
出典メモuspto-grants-1997_04