반응 #8526

반응 방정식

hydrogen

2,3, 4-Trifluoronitrobenzene

methyl pyruvate

magnesium sulfate

→

title compound

수율 97.4%

Methyl 2-(2,3,4-trifluoroanilino)propionate

수율 97.4%

용매

methanol

반응 조건

후처리

1. 1
   기타Then the liquid reaction mixture
2. 2
   여과was filtered through celite
3. 3
   농축The obtained filtrate was concentrated under reduced pressure and Florisil (100 g) and diethyl ether (700 ml)
4. 4
   workup.ADDITIONwere added to the residue
5. 5
   기타the liquid reaction mixture
6. 6
   여과was filtered
7. 7
   기타The obtained organic layer was evaporated
8. 8
   기타the crystals thus precipitated
9. 9
   여과were filtered
10. 10
    세척while washing with hexane

실험 절차

2,3, 4-Trifluoronitrobenzene (100 g) and methyl pyruvate (57.6 g) were dissolved in methanol (1000 ml). After adding 5% Pd—C (20.0 g) and anhydrous magnesium sulfate (90 g), the mixture was stirred at room temperature in a hydrogen atmosphere for 16 hours. Then the liquid reaction mixture was filtered through celite to thereby eliminate Pd—C and magnesium sulfate. The obtained filtrate was concentrated under reduced pressure and Florisil (100 g) and diethyl ether (700 ml) were added to the residue. After stirring for 2 hours, the liquid reaction mixture was filtered. The obtained organic layer was evaporated and the crystals thus precipitated were filtered while washing with hexane. Thus the title compound (128.2 g) was obtained as slightly yellowish crystals.

출처