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HRID 1359349作成日:2026年10月26日

Dimethylformamide → 2-benzyl-6-[(3S,4R)-3-chloro-4-methoxypyrrolidine-1-yl]-3-iodopyridine

https://huagongshe.com/reaction/1359349

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Lithium ChlorideHCID 433294—
反応物2-benzyl-6-((3R,4R)-3-(3-nitrobenzenesulfonyl)oxy-4-methoxypyrrolidine-1-yl]-3-iodopyridineHCID 87983359—
溶媒WaterHCID 962—
生成物2-benzyl-6-[(3S,4R)-3-chloro-4-methoxypyrrolidine-1-yl]-3-iodopyridineHCID 6975863448.9%

反応条件

温度75 °C

反応手順

A mixture of 553 g of 2-benzyl-6-((3R,4R)-3-(3-nitrobenzenesulfonyl)oxy-4-methoxypyrrolidine-1-yl]-3-iodopyridine, 79 mg of lithium chloride and 5.0 ml of N,N-dimethylformamide was heated under stirring at 75° C. for 9 hours. After cooling as it was, water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic phase was washed with water and brine, and the solvent was removed. The residue was subjected to NH-silica gel (Fuji Silicia) column chromatography and eluted with hexane/ethyl acetate (10:1) and then with hexane/ethyl acetate (5:1), to give 391 mg of the target compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06599917B1
出典データセットuspto-grants-2003_07
ORD IDord-b70343027b144a6aa50a9dc31dfafa60
出典メモuspto-grants-2003_07