Reaktion #357770

Reaktionsgleichung

2-chloro-6-methyl-4-(trifluoromethyl)pyridine

piperazine

triethylamine

→

desired product

Ausbeute 70.2%

1-[6-Methyl-4-(trifluoromethyl)pyridin-2-yl]piperazine

Ausbeute 70.2%

Lösungsmittel

1,4-dioxane

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate three times
2. 2
   Trocknendried with sodium sulfate
3. 3
   Filtrationfiltered
4. 4
   Einengenconcentrated in vacuo
5. 5
   SonstigeThe crude residue was purified by flash column chromatography (10% MeOH/5% Et3N/EtOAc)

Vorschrift

A solution of 2-chloro-6-methyl-4-(trifluoromethyl)pyridine (1.0 g, 5.11 mmol), piperazine (1.32 g, 15.3 mmol), and triethylamine (0.71 mL, 5.1 mmol) were mixed in 1,4-dioxane (10 mL). After stirring at 100° C. for 5 h, the reaction solution was diluted with water and extracted with ethyl acetate three times, dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by flash column chromatography (10% MeOH/5% Et3N/EtOAc) to yield the desired product (880 mg, 70.2%). LCMS calculated for C11H15F3N3: (M+1) 246.1; found 246.1.

Quelle