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HRID 415977作成日:2026年10月26日

Ammonium Chloride → 1-Cyclohexyl-3-(2,6-dichloro-4-methoxy-benzyl)-pyrrolidin-2-one

https://huagongshe.com/reaction/415977

反応式

関与物質

役割名称HCID仕込み量
反応物Ammonium ChlorideHCID 25517—
反応物N-Cyclohexyl-2-pyrrolidoneHCID 81278—
反応物Lithium diisopropylamideHCID 2724682—
反応物2-(Bromomethyl)-1,3-dichloro-5-methoxybenzeneHCID 59299479—
溶媒TetrahydrofuranHCID 8028—
生成物1-Cyclohexyl-3-(2,6-dichloro-4-methoxy-benzyl)-pyrrolidin-2-oneHCID 5929941469%

反応条件

温度-78 °C

反応手順

Dissolve commercially available 1-cyclohexyl-pyrrolidin-2-one (88.2 g, 527.9 mmol) in 2500 mL tetrahydrofuran and cool to −78° C. Add 176 mL 2 M LDA and stir for ˜5 min. Add 2-bromomethyl-1,3-dichloro-5-methoxy-benzene (95 g, 351.9 mmol) and allow the reaction to warm to room temperature. Pour the mixture into saturated ammonium chloride and extract twice with dichloromethane. Dry over sodium sulfate, filter and concentrate under vacuum to obtain a tan solid. Add hexanes and stir rapidly before filtering. Wash the filter cake several times with cold hexane to obtain 86 g (69%) of a light-tan solid: MS (m/z): 356 (M+).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08088776B2
出典データセットuspto-grants-2012_01
ORD IDord-671ed090c526489ea143d527e9a47bc2
出典メモuspto-grants-2012_01