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HRID 69056作成日:2026年10月26日

Potassium Carbonate → 1-Ethyl-3,3,5-trimethyl-7-[3-(2-phenyl-benzoimidazol-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione hydrochloride

https://huagongshe.com/reaction/69056

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物2-PhenylbenzimidazoleHCID 12855—
反応物Ethanol hydrochlorideHCID 21887872—
反応物1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dioneHCID 68672792—
溶媒IsopropanolHCID 3776—
溶媒DimethylformamideHCID 6228—
生成物1-Ethyl-3,3,5-trimethyl-7-[3-(2-phenyl-benzoimidazol-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione hydrochlorideHCID 70656674—

反応条件

温度60 °C

反応手順

2-Phenyl-1H-benzimidazole (0.2 g) and potassium carbonate (0.29 g) were added to a DMF solution (5 ml) of 1-ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.49 g). The mixture was stirred at 60° C. for 7 hours. The reaction mixture was poured to ice water (50 ml), and the generated insoluble matter was separated. The insoluble matter was dissolved in ethyl acetate. The liquid was dried over sodium sulfate and condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3). The purified product was condensed under reduced pressure. A 1N-hydrogen chloride ethanol solution (1.0 ml) was added to an isopropyl alcohol solution of the residue. The mixture was condensed under reduced pressure. Ether was added to the residue. The generated insoluble matter was separated by filtration and dried to give the title compound (0.32 g) as a white powder.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08822453B2
出典データセットuspto-grants-2014_09
ORD IDord-de8ab4288e134fb39d21852ded4f2ecc
出典メモuspto-grants-2014_09