反应 #8526

反应方程式

hydrogen

2,3, 4-Trifluoronitrobenzene

methyl pyruvate

magnesium sulfate

→

title compound

收率 97.4%

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

收率 97.4%

溶剂

methanol

反应条件

后处理

1. 1
   其他Then the liquid reaction mixture
2. 2
   过滤was filtered through celite
3. 3
   浓缩The 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
   其他the liquid reaction mixture
6. 6
   过滤was filtered
7. 7
   其他The obtained organic layer was evaporated
8. 8
   其他the crystals thus precipitated
9. 9
   过滤were filtered
10. 10
    洗涤while washing with hexane

实验过程

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.

来源