반응 #8527

ord-3aa39437285a4e61ad16bed02546d92a

반응 방정식

[H][H]
hydrogen
Nc1ccc(F)c(F)c1F
2,3,4-Trifluoroaniline
COC(=O)C(C)=O
methyl pyruvate
O=S(=O)([O-])[O-].[Mg+2]
magnesium sulfate
COC(=O)C(C)Nc1ccc(F)c(F)c1F
title compound
수율 95.3%
COC(=O)C(C)Nc1ccc(F)c(F)c1F
Methyl 2-(2,3,4-trifluoroanilino)propionate
수율 95.3%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After filtering off Pd—C and magnesium sulfate
  2. 2
    농축the obtained filtrate was concentrated under reduced pressure
  3. 3
    기타The crystals thus precipitated
  4. 4
    여과were filtered
  5. 5
    세척while washing with hexane

실험 절차

2,3,4-Trifluoroaniline (2.94 g) and methyl pyruvate (2.04 g) were dissolved in methanol (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 crystals thus precipitated were filtered while washing with hexane. Thus the title compound (4.44 g) was obtained as slightly yellowish crystals. Various spectral data of this product was identical with those obtained in Example 5.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087778B2uspto-grants-2006_08