反应详情

(Step 2) To a suspension of lithium aluminum hydride (1.56 g) in tetrahydrofuran (250 ml) was added a solution of 5-chloro-2-[(1-methylethyl)sulfanyl]benzonitrile obtained in Step 1 (7.25 g) in tetrahydrofuran (50 ml) 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 30 min, and the inorganic substance was filtered off through celite. The filtrate was concentrated under reduced pressure. The residue was dissolved in methanol, 4N hydrogen chloride-ethyl acetate solution (15 ml) was added, and the solvent was evaporated under reduced pressure. The obtained solid was washed with a mixed solvent of diisopropyl ether-ethyl acetate to give 1-{5-chloro-2-[(1-methylethyl)sulfanyl]phenyl}methanamine hydrochloride (6.57 g).

1. stirringThe mixture was further stirred at room temperature for 30 min
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 (15 ml) was added
6. customthe solvent was evaporated under reduced pressure
7. washThe obtained solid was washed with a mixed solvent of diisopropyl ether-ethyl acetate