反応 #70452

反応方程式

triethylamine hydrochloride

Triethylamine

6-chloro-nicotinonitrile

(R)-2-methyl-piperazine

→

desired product

収率 59.0%

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

収率 59.0%

溶媒

DMF

EtOAc

Water

反応条件

後処理

1. 1
   その他the organic layer is separated
2. 2
   乾燥dried over sodium sulfate
3. 3
   濃縮concentrated under reduced pressure to a white residue
4. 4
   その他The solid is further dried under high vacuum

実験手順

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%).

出典