Reaktion #5972

Reaktionsgleichung

methyl 2-chloro-5a,6,7, 8,9,9a-hexahydrodibenzofuran-4-carboxylate

→

2-Chloro-5a,6,7,8,9,9a-Hexahydrodibenzofuran-4 -Carboxylic Acid

Lösungsmittel

methanol

sodium hydroxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThis is cooled
2. 2
   Sonstigethe methanol is removed under vacuo
3. 3
   workup.ADDITIONdiluted with 30 ml water
4. 4
   Filtrationfiltered
5. 5
   Extraktionextracted with ethyl acetate
6. 6
   Waschenwashed with water
7. 7
   Trocknendried over magnesium sulfate
8. 8
   Sonstigeevaporated to dryness
9. 9
   Sonstigeto give crystalline product which

Vorschrift

A mixture of 1.6 g of methyl 2-chloro-5a,6,7, 8,9,9a-hexahydrodibenzofuran-4-carboxylate in 10 ml of methanol and 20 ml of 1N sodium hydroxide is stirred at 50° C. for 6 hours. This is cooled, the methanol is removed under vacuo, diluted with 30 ml water and filtered. The aqueous solution is acidified with acetic acid, extracted with ethyl acetate, washed with water, dried over magnesium sulfate and evaporated to dryness to give crystalline product which is used directly in the next step.

Quelle