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HRID 926031作成日:2026年10月27日

Dichloromethane → HCID 178501248、化合物

https://huagongshe.com/reaction/926031

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 178501210HCID 178501210—
溶媒PyridineHCID 1049—
生成物HCID 178501248HCID 17850124892.3%

反応手順

A mixture of 604 mg of methyl trans-4-aminocyclohexane 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, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 1.27 g of 2-(trimethylsilyl)ethyl 3-{[trans-4-(methoxycarbonyl)cyclohexyl]sulfamoyl}benzoate as a colorless oily substance.

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-2db04d9ff51841d99a32c28be3946c70
出典メモuspto-grants-2016_03