Reaktion #612083

Reaktionsgleichung

1-methylpiperazine

2,4-dichloro-5-nitro-pyridine

DIPEA

→

1-(2-chloro-5-nitro-4-pyridyl)-4-methyl-piperazine

Lösungsmittel

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was partitioned between ethyl acetate and NaHCO3 (sat. aq. soln)
2. 2
   WaschenThe combined organics was washed with brine
3. 3
   Trocknendried over MgSO4
4. 4
   Einengenconcentrated under reduced pressure

Vorschrift

1-methylpiperazine (119.3 mg, 132.6 μL, 1.191 mmol) in THF (1.5 mL) was added to a stirred solution of 2,4-dichloro-5-nitro-pyridine (200 mg, 1.036 mmol) and DIPEA (160.6 mg, 216.4 μL, 1.243 mmol) in THF (3.000 mL) at 0° C. under an atmosphere of nitrogen. The reaction was allowed to stir at ambient temperature overnight. The reaction mixture was partitioned between ethyl acetate and NaHCO3 (sat. aq. soln). The combined organics was washed with brine, dried over MgSO4 and concentrated under reduced pressure to yield 1-(2-chloro-5-nitro-4-pyridyl)-4-methyl-piperazine. (100%) MS (ES+) 257.1.

Quelle