C([N:8]1[CH2:13][CH2:12][N:11]([CH:14]([CH3:16])[CH3:15])[CH2:10][C@@H:9]1[CH3:17])(OC(C)(C)C)=O.Cl>O1CCOCC1>[CH:14]([N:11]1[CH2:12][CH2:13][NH:8][C@@H:9]([CH3:17])[CH2:10]1)([CH3:16])[CH3:15]To crude (S)-1-Boc-2-methyl-4-isopropylpiperazine in 1,4-dioxane (10 mL) was added HCl (5 mL of a 4M solution in 1,4-dioxane). The reaction mixture was stirred at room temperature for 28 h then concentrated. The resulting solid was suspended in diethyl ether, concentrated and dried on high vacuum for 1 d. The resulting solid was taken up in aq. 2N NaOH and the solution extracted three times with DCM. The combined organic layers were dried over sodium sulfate, filtered, and concentrated to provide the free base of the product which was used without further purification. LCMS-ESI+: calc'd for C8H18N2 (M+H+): 143.1; Found: 143.7 (M+H+).
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