反应 #8528

ord-ef41386ffd2e4542a863081859790979

反应方程式

[H][H]
hydrogen
O=[N+]([O-])c1ccc(F)c(F)c1F
2,3,4-Trifluoronitrobenzene
COC(=O)C(C)=O
methyl pyruvate
CCO
ethanol
O=S(=O)([O-])[O-].[Mg+2]
magnesium sulfate
CCOC(=O)C(C)Nc1ccc(F)c(F)c1F
title compound
CCOC(=O)C(C)Nc1ccc(F)c(F)c1F
Ethyl 2-(2,3,4-trifluoroanilino)propionate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤After filtering off Pd—C and magnesium sulfate
  2. 2
    浓缩the obtained filtrate was concentrated under reduced pressure
  3. 3
    其他The residue thus obtained

实验过程

2,3,4-Trifluoronitrobenzene (3.54 g) and methyl pyruvate (2.32 g) were dissolved in ethanol (30 ml). After adding 5% Pd—C (2.0 g) and anhydrous magnesium sulfate (2.65 g), the mixture was stirred at 50° C. in a hydrogen atmosphere for 16 hours. After filtering off Pd—C and magnesium sulfate, the obtained filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography (ethyl acetate-normal hexane=1:4) to give the title compound (4.84 g) as a pale yellow oily substance.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07087778B2uspto-grants-2006_08