Reaktion #1120021

Reaktionsgleichung

sodium

methyl 1-acetylamino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylate

→

1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid

Lösungsmittel

sodium hydroxide

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued at 60° C. overnight
3. 3
   SonstigeThe methanol is removed in vacuum
4. 4
   workup.ADDITIONdiluted with water
5. 5
   Filtrationfiltered
6. 6
   Filtrationfiltered
7. 7
   Waschenwashed with water
8. 8
   Trocknendried over magnesium sulfate
9. 9
   Sonstigeevaporated to dryness

Vorschrift

To a solution of 0.3 g of sodium in 15 ml methanol is added 0.6 g of methyl 1-acetylamino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylate. Stirring is continued at 60° C. for two days. This is then diluted with 5 ml 1N sodium hydroxide and stirring continued at 60° C. overnight. The methanol is removed in vacuum, diluted with water, filtered, acidified with acetic acid, filtered, washed with water, dried over magnesium sulfate and evaporated to dryness to obtain 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid. This is purified by crystallization from ethyl acetate/ether.

Quelle