Reaktion #669908

Reaktionsgleichung

ethyl 2-oxobicyclo[3.1.0]hexane-6-carboxylate

hydrochloric acid

→

title compound

2-Oxobicyclo[3.1.0]hexane-6-carboxylic acid

Lösungsmittel

sodium hydroxide

Reaktionsbedingungen

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 1 N 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. FDMS: m/z =140 (M+) Analysis calculated for C7H8O3 : C, 60.00; H, 5.75. Found: C, 60.14; H, 5.79.

Quelle