반응 #674767

반응 방정식

water

4-(benzyloxy)aniline

2-chloro-5-fluoro-3-nitropyridine

K2CO3

→

title compound

수율 24.3%

N2-[4-(benzyloxy)phenyl]-5-fluoropyridine-2,3-diamine

수율 24.3%

용매

EtOH

DMF

반응 조건

후처리

1. 1
   추출extracted with AcOEt
2. 2
   건조The organic layer was dried over MgSO4
3. 3
   농축concentrated in vacuo
4. 4
   여과collected by filtration
5. 5
   기타The solid obtained
6. 6
   workup.STIRRINGUnder H2 atmosphere, the mixture was stirred for 1 h
7. 7
   여과filtered
8. 8
   기타evaporated
9. 9
   기타The residue was chromatographed on silica gel eluting with Hexane/AcOEt

실험 절차

A mixture of 4-(benzyloxy)aniline (2.26 g), 2-chloro-5-fluoro-3-nitropyridine (2 g) and K2CO3 (3.13 g) in DMF (20 mL) was stirred at 120° C. for 5 h, treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was suspended in IPE and collected by filtration. The solid obtained above was dissolved in EtOH (20 mL), and Pt/C (2 g) was added. Under H2 atmosphere, the mixture was stirred for 1 h, filtered and evaporated. The residue was chromatographed on silica gel eluting with Hexane/AcOEt to give the title compound (0.85 g).

출처