Piperazine → HCID 57808432, compound

Participants

Reaction Steps

An oven-dried, nitrogen purged flask was charged with 124 mg LiAlH4 (3.26 mmol) and suspended in 2.0 mL anhydrous THF. Diketopiperazine 11 (200 mg, 1.09 mmol) was added dropwise as a solution in 7.0 mL anhydrous THF. The reaction was stirred at room temperature for 1.5 hours, followed by heating at 40° C. for 5 hours. The reaction was allowed to cool to room temperature, diluted with ca. 10 mL diethyl ether, quenched with sequential addition of 60 μL H2O, 120 μL 10% NaOH, 180 μL H2O, and the resulting aluminum salts filtered off. The organic solution was dried over MgSO4 and evaporated to dryness under reduced pressure to yield 140 mg (82% yield) of product piperazine as a slightly brown oil which was used immediately without further purification. MS (ESI-TOF) MH+ expected: 157.1699, found: 157.1703.

Provenance & Evidence