Reaktion #70452

Reaktionsgleichung

triethylamine hydrochloride

Triethylamine

6-chloro-nicotinonitrile

(R)-2-methyl-piperazine

→

desired product

Ausbeute 59.0%

6-((R)-3-Methyl-piperazin-1-yl)-nicotinonitrile

Ausbeute 59.0%

Lösungsmittel

DMF

EtOAc

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe organic layer is separated
2. 2
   Trocknendried over sodium sulfate
3. 3
   Einengenconcentrated under reduced pressure to a white residue
4. 4
   SonstigeThe solid is further dried under high vacuum

Vorschrift

Triethylamine (5.51 g, 4 mL, 54.6 mmol, 2.7 eq) is added to a solution of 6-chloro-nicotinonitrile (2.76 g, 20 mmol, 1 eq), (R)-2-methyl-piperazine (2.00 g, 20 mmol, 1 eq) in DMF (15 mL), and the resulting solution is stirred at rt for 36 h. A white precipitate of triethylamine hydrochloride forms in the course of the reaction. Water (15 mL) and EtOAc (100 mL) are added, the organic layer is separated, dried over sodium sulfate and concentrated under reduced pressure to a white residue. The solid is further dried under high vacuum to yield the desired product as a white solid (2.3 g, 59%).

Quelle