Reaktion #57667

ord-3ef1fbba0152493389dc72a283a63524

Reaktionsgleichung

CCOC(=O)c1oc2c(Cl)cc(Cl)c(O)c2c1C
5,7-dichloro-4-hydroxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester
CI
iodomethane
O=C([O-])[O-].[K+].[K+]
K2CO3
CCOC(=O)c1oc2c(Cl)cc(Cl)c(OC)c2c1C
5,7-dichloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester
Ausbeute 99.3%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe mixture was washed with brine
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe combined ethyl acetate solution was washed with brine
  4. 4
    SonstigeRemoval of the solvent in vacuo

Vorschrift

To 120 mg of 5,7-dichloro-4-hydroxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester was added 1 mL of iodomethane, 200 mg of K2CO3 and 4 mL of DMF. The mixture was stirred at room temperature overnight. The mixture was washed with brine and extracted with ethyl acetate. The combined ethyl acetate solution was washed with brine. Removal of the solvent in vacuo gave 125 mg (99% yield) of 5,7-dichloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester as off-white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07420001B2uspto-grants-2008_09