Water → 2-(2,6-Dimethyl-phenyl)4-methyl-5-nitro-pyridine

Temperatur

110 °C

A mixture of 2,6-dimethylphenylboronic acid (6.5 g, 43.5 mmol), 2-chloro-4-methyl-5-nitro-pyridine (5 g, 28.9 mmol), Pd(PPh3)4, (1.5 g, 1.5 mmol), Na2CO3 (4.6 g, 43.5 mm water (20 mL), and EtOH (5 mL) is heated in a sealed tube under nitrogen at 110° C. for 18 hours. The mixture is cooled to room temperature, diluted with EtOAc (150 mL), washed with saturated solution of Na2CO3 (50 mL 3×), water (50 mL) and brine (50 mL), dried (Na2SO4), and concentrated under reduced pressure. The residue is purified by chromatography on silica gel (Hexane/EtOAc, 6:1) to afford 2-(2,6-dimethyl-phenyl)-4-methyl-5-nitro-pyridine as a colorless oil.

1. temperatureThe mixture is cooled to room temperature
2. washwashed with saturated solution of Na2CO3 (50 mL 3×), water (50 mL) and brine (50 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customThe residue is purified by chromatography on silica gel (Hexane/EtOAc, 6:1)

ORD-Eintrag

ord-8405865ab2ca428dac4aa38ec0ba3e14

Quelldatensatz

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07906528B2