Aluminium lithium hydride → (2R)-2-butylpiperazine

関与物質

反応手順

To a cooled to −78° C. solution of (3R)-3-butyl-2,5-piperazinedione from step (b) above (600 mg, 2.52 mmol) in THF (10 mL) was added dropwise lithium aluminum hydride (21 mL, 21.1 mmol, 1M in THF, Aldrich). The mixture was stirred at room temperature for 1 h, and then heated at reflux for 16 h. The mixture was cooled to 0° C. and quenched with sodium sulfate decahydrate until the gas evolution ceased. The mixture was stirred at room temperature for 3 h, filtered and the filter cake was washed with THF (2×10 mL). The filtrate was concentrated in vacuo to give the title compound as a yellow solid. MS (ESI, positive ion) m/z: 143 (M+1).

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