Reaktion #44188

ord-b22fa8f5e6e24492a355700c274d8c47

Reaktionsgleichung

CCOC(=O)c1cn(C)c(=O)cc1Cl
4-chloro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid ethyl ester
O=C1CCC(=O)N1Cl
NCS
CCOC(=O)c1cn(C)c(=O)c(Cl)c1Cl
4,5-dichloro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid ethyl ester
Ausbeute 95.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with 0.1 N HCl solution
  2. 2
    TrocknenThe organic layer was dried (MgSO4)
  3. 3
    Einengenconcentrated under reduced pressure

Vorschrift

A mixture of 4-chloro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid ethyl ester (1.00 g, 4.64 mmol) and NCS (0.68 g, 5.10 mmol) in DMF (30 mL) was stirred for 1 hour. The reaction mixture was diluted with EtOAc and washed with 0.1 N HCl solution. The organic layer was dried (MgSO4) and concentrated under reduced pressure to give 1.10 g (95%) of 4,5-dichloro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid ethyl ester.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732616B2uspto-grants-2010_06