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HRID 1041845作成日:2026年10月25日

Dichloromethane → (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate

https://huagongshe.com/reaction/1041845

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物Methyl triflateHCID 9526—
反応物3-Cyano-4-dimethylamino-benzoic acid methyl esterHCID 59847657—
溶媒Diethyl EtherHCID 3283—
生成物(2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonateHCID 8662151969%

反応手順

To a stirred solution of 6.16 g (30.2 mmol) 3 and 110 ml dichloromethane were added 50.0 g (302 mmol) methyltriflate (Aldrich) drop wisely. The reaction mixture was stirred over night and diethylether was added. After evaporation of one third of the solvent volume the desired compound precipitates and the rest of the solvent were decanted. The solid was washed extensively (ten times) with large amounts of diethylether. The solid was dried by use of oil pump vacuum and purified by (C-18) RP-column chromatography (acetonitril/water—gradient 1:99 to 80:20). The desired compound 4 was obtained in 69% yield (20.8 mmol, 7.68 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08557776B2
出典データセットuspto-grants-2013_10
ORD IDord-14848f56a14a460f8cd5383286b8ca90
出典メモuspto-grants-2013_10