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HRID 1013975作成日:2026年10月27日

Sodium sulfate decahydrate → 1-[3-Chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride

https://huagongshe.com/reaction/1013975

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium sulfate decahydrateHCID 62649—
反応物Aluminium lithium hydrideHCID 21226445—
反応物3-Chloro-5-(methylthio)benzonitrileHCID 66878686—
溶媒TetrahydrofuranHCID 8028—
生成物1-[3-Chloro-5-(methylsulfanyl)phenyl]methanamine hydrochlorideHCID 66877840143.4%

反応手順

(Step 2) To a suspension of lithium aluminum hydride (0.79 g) in tetrahydrofuran (200 ml) was added 3-chloro-5-(methylsulfanyl)benzonitrile obtained in Step 1 (3.2 g) at 0° C. The mixture was stirred at room temperature for 3 hr, and treated with sodium sulfate 10 hydrate. The mixture was stirred at room temperature for 30 min, and the inorganic substance was filtered off through celite. The filtrate was concentrated under reduced pressure. The residue was dissolved in methanol, and 4N hydrogen chloride-ethyl acetate solution (5 ml) was added. The mixture was crystallized from methanol-ethyl acetate, and the obtained crystals were washed with ethyl acetate to give 1-[3-chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride (2.8 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07982044B2
出典データセットuspto-grants-2011_07
ORD IDord-e2751b74a1d1420681dfe601e99120eb
出典メモuspto-grants-2011_07