Reaktion #1562928

ord-92ecb827f70f4adf8c7660d74bd05f36

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeevaporated
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in 300 ml of a 0.1 M aqueous solution of sodium hydroxide
  3. 3
    Waschenwashed three times with 50 ml each of diisopropyl ether
  4. 4
    workup.STIRRINGthe mixture stirred for 30 min at room temperature
  5. 5
    FiltrationThe product was collected by filtration
  6. 6
    Waschenwashed
  7. 7
    Sonstigedried in vacuo

Vorschrift

4.5 g of 7-(2-m-tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic acid 2-m-tolyl-ethyl ester and 650 mg of sodium hydroxide were dissolved in 50 ml of methanol, 50 ml of THF and 5 ml of water. The mixture was kept at room temperature for 20 h, then stirred at 50° C. for 5 h and evaporated. The residue was dissolved in 300 ml of a 0.1 M aqueous solution of sodium hydroxide and washed three times with 50 ml each of diisopropyl ether. The pH was adjusted to 2 with sodium hydrogensulfate and the mixture stirred for 30 min at room temperature. The product was collected by filtration, washed and dried in vacuo to yield 3.1 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09018383B2uspto-grants-2015_04