Piperazine → 1-(4-Methyl-3-nitrophenyl)piperazine

Temperatur

110 °C

palladium(II) acetate (0.065 g, 0.29 mmol), BINAP (0.144 g, 0.23 mmol) and CS2CO3 (0.943 g, 2.89 mmol) were added to a mixture of 4-bromo-1-methyl-2-nitrobenzene (0.5 g, 2.31 mmol) and piperazine (1.623 g, 18.84 mmol) . The suspension were heated to 110 °C for 24 hours, LCMS showed product mass [M+1]: 222.1 at retension time RT=1.21 min (polar short purity method). Workup reaction by additional of water (10mL), extracted with EtOAc (3x20 mL), washed with brine, dried with Na2SO4, evaporated off solvent to give a residue, which was purified by isco chromatographer, eluting with 0-10% MeOH in DCM to give 1-(4-methyl-3-nitrophenyl)piperazine (0.201 g, 39.3 %) as a yellow solid.

ORD-Eintrag

ord-7a7d88bb15974f808c2ac9e73fb46a04

Quelldatensatz

750 AstraZeneca ELN dataset

Originallink

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