반응 #5524

ord-aac0c1f80f444f1e85571cb9c0058d96

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 4 hours
  2. 2
    기타After the solvent was removed
  3. 3
    workup.ADDITIONchloroform was added to the residue, which
  4. 4
    세척was washed in turn with saturated sodium bicarbonate and saturated saline
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    농축After the solvent was concentrated
  7. 7
    workup.ADDITIONn-hexane was added to the mixture
  8. 8
    기타Then, the crystals precipitated
  9. 9
    여과were filtered off
  10. 10
    세척washed with n-hexane

실험 절차

A solution of 2-amino-6-chloropyridine (6.43 g, 50 mmoles) and ethyl bromopyruvate (9.75 g, 50 mmoles) in ethanol (150 ml) was heated at reflux for 4 hours. After the solvent was removed, chloroform was added to the residue, which was washed in turn with saturated sodium bicarbonate and saturated saline, and then dried over anhydrous magnesium sulfate. After the solvent was concentrated, n-hexane was added to the mixture. Then, the crystals precipitated were filtered off and washed with n-hexane to obtain 7.60 g of the desired product (67.6%, pale yellow crystals).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05244908uspto-grants-1993_09