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HRID 926034作成日:2026年10月26日

Dichloromethane → HCID 178501219、化合物

https://huagongshe.com/reaction/926034

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物TriethylamineHCID 8471—
反応物2-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoateHCID 86676334—
反応物HCID 178501217HCID 178501217—
溶媒PyridineHCID 1049—
生成物HCID 178501219HCID 17850121920.7%

反応手順

A mixture of 734 mg of methyl trans-4-(isopropylamino)cyclohexane carboxylate hydrochloride, 0.90 mL of triethylamine, and 10 mL of dichloromethane was stirred at room temperature for 30 minutes, and 10 mL of pyridine and 1.00 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate were added thereto in this order, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and to the residue was added an aqueous citric acid solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 311 mg of 2-(trimethylsilyl)ethyl 3-{isopropyl[trans-4-(methoxycarbonyl)cyclohexyl]sulfamoyl}benzoate as a pale yellow solid. ESI+: 484

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09284295B2
出典データセットuspto-grants-2016_03
ORD IDord-eb94420c38534867907ca8e7dd4952e8
出典メモuspto-grants-2016_03