Reaktion #163102

Reaktionsgleichung

2,3,5,6-tetrachloropyridine

5-cyclopropyl-1H-pyrazol-3-amine

triethylamine

→

title compound

Ausbeute 12.8%

3,5,6-Trichloro-N-(5-cyclopropyl-1H-pyrazol-3-yl)pyridin-2-amine

Ausbeute 12.8%

Lösungsmittel

NMP

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigequenched with water (10 ml)
2. 2
   Extraktionextracted with MTBE (4×30 ml)
3. 3
   SonstigeThe combined organic fractions were then dried
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated
6. 6
   SonstigeThe resulting solid was purified by column chromatography (DCM-MeOH=50:1)

Vorschrift

A solution of 2,3,5,6-tetrachloropyridine (0.20 g, 0.9 mmol), 5-cyclopropyl-1H-pyrazol-3-amine (0.20 g, 1.8 mmol), and triethylamine (0.10 g, 1.4 mmol) in NMP (2 ml) was heated in a microwave at 200° C. for 30 min. The reaction was cooled to 25° C., quenched with water (10 ml), and extracted with MTBE (4×30 ml). The combined organic fractions were then dried, filtered, and concentrated. The resulting solid was purified by column chromatography (DCM-MeOH=50:1) to give the title compound (0.035 g, 12%). MS: Calcd.: 303. Found: [M+H]+ 303.

Quelle