Reaktion #1862

ord-07beb0ec388f43cd9ac71486ee726a73

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    ExtraktionThe resulting solution was extracted with ethyl acetate
  2. 2
    TrocknenThe extracts were dried over magnesium sulfate
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigeto give 49.1 g (98%) of the crude material
  6. 6
    SonstigeRecrystallization from 100 ml of ethyl acetate

Vorschrift

A mixture of 60 g of ethyl 2-oxobicyclo[3.1.0]hexane-6-carboxylate and 300 ml of 1N sodium hydroxide was stirred at 25°-30° C. After 2.5 hours, concentrated hydrochloric acid was added to adjust the pH to 0.8-1.2. The resulting solution was extracted with ethyl acetate. The extracts were dried over magnesium sulfate, filtered, and concentrated to give 49.1 g (98%) of the crude material. Recrystallization from 100 ml of ethyl acetate gave the title compound, mp 123.5°-128° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05726320uspto-grants-1998_03