반응 #167717

반응 방정식

2-amino-3,5-dibromopyrazine

2-chloro-3,6-difluorobenzylamine

N, N-diethylisopropylamine

→

5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine

수율 70.0%

용매

n-BuOH

반응 조건

후처리

1. 1
   기타After volatile components were removed on rotavap
2. 2
   workup.ADDITIONEtOAc and water were added to the residue
3. 3
   추출the extraction
4. 4
   기타dried
5. 5
   농축concentrated

실험 절차

A solution of 2-amino-3,5-dibromopyrazine (29 mmol, 7.35 g), 2-chloro-3,6-difluorobenzylamine (29 mmol, 5.16 g), and N, N-diethylisopropylamine (32 mmol, 5.6 mL) in n-BuOH (20 mL) was refluxed for 72 hrs. After volatile components were removed on rotavap, EtOAc and water were added to the residue to facilitate the extraction. The combined organic layers were combined, dried, concentrated, and then subjected to a silica gel column chromatography by using hexanes/EtOAc (4:1) as eluents, furnishing 5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine in 70% yield (7.14 g).

출처