Reaktion #2005516

ord-815eaa6f7c864670a42d42630158ea6b

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed in vacuo
  2. 2
    workup.DISSOLUTIONthe residue dissolved in 200 ml of water
  3. 3
    SonstigeThe organic layer was separated
  4. 4
    Waschenwashed with 100 ml of a saturated aqueous sodium carbonate solution
  5. 5
    Trocknendried with magnesium sulfate
  6. 6
    Sonstigeevaporated

Vorschrift

2.5 g of 7-hydroxy-benzo[1,3]dioxole-5-carboxylic acid, 6.8 g of 1-(2-bromo-ethyl)-3-methyl-benzene and 7.6 g of potassium carbonate were stirred in 100 ml of anhydrous DMF for 10 h at 80° C. Then another 1.4 g of 1-(2-bromo-ethyl)-3-methyl-benzene and 1.5 g of potassium carbonate were added and the mixture was stirred for 5 h at 90° C. The solvent was removed in vacuo and the residue dissolved in 200 ml of water and 200 ml of EA. The organic layer was separated, washed with 100 ml of a saturated aqueous sodium carbonate solution, dried with magnesium sulfate and evaporated to yield 4.5 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08618304B2uspto-grants-2013_12