反应详情

(Step 2) To a suspension of lithium aluminum hydride (1.41 g) in tetrahydrofuran (300 ml) was added 5-chloro-2-(methylsulfanyl)benzonitrile obtained in Step 1 (5.7 g) at 0° C. The mixture was stirred at room temperature for 3 hr, and treated with sodium sulfate 10 hydrate. The mixture was further stirred at room temperature for 1 hr, 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 (10 ml) was added. The mixture was crystallized from methanol-ethyl acetate to give 1-[5-chloro-2-(methylsulfanyl)phenyl]methanamine hydrochloride (5.11 g).

1. stirringThe mixture was further stirred at room temperature for 1 hr
2. filtrationthe inorganic substance was filtered off through celite
3. concentrationThe filtrate was concentrated under reduced pressure
4. dissolutionThe residue was dissolved in methanol
5. addition4N hydrogen chloride-ethyl acetate solution (10 ml) was added
6. customThe mixture was crystallized from methanol-ethyl acetate