반응 #70451

반응 방정식

triethylamine hydrochloride

Triethylamine

6-chloro-nicotinonitrile

(S)-2-methyl-piperazine

→

desired product

수율 69.2%

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

수율 69.2%

용매

DMF

EtOAc

Water

반응 조건

후처리

1. 1
   기타the organic layer is separated
2. 2
   건조dried over sodium sulfate
3. 3
   농축concentrated under reduced pressure to a white residue
4. 4
   기타The solid is further dried under high vacuum

실험 절차

Triethylamine (4.13 g, 3 mL, 40.8 mmol, 4 eq) is added to a solution of 6-chloro-nicotinonitrile (1.38 g, 10 mmol, 1 eq), (S)-2-methyl-piperazine (1.00 g, 10 mmol, 1 eq) in DMF (15 mL), and the resulting solution is stirred at rt for 14 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 (1.4 g, 69%).

출처