Reaktion #348721

Reaktionsgleichung

2-ethyl-6-chloro-2-methyl-α-oxo-5-indanacetic acid methyl ester

hydrogen

→

2-ethyl-6-chloro-2-methyl-5-indanacetic acid methyl ester

Lösungsmittel

sulphuric acid

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis hydrogenated at 45°
2. 2
   FiltrationAfter the take up of the theoretic amount of hydrogen the catalyst is filtered off
3. 3
   workup.ADDITIONthe solution is diluted with a 5% sodium bicarbonate solution
4. 4
   Extraktionextracted with ether
5. 5
   WaschenThe extract is washed with water
6. 6
   Trocknendried over sodium sulphate
7. 7
   Einengenconcentrated by evaporation
8. 8
   SonstigeThe resulting title compound is purified by chromatography

Vorschrift

A solution of 5.2 g of 2-ethyl-6-chloro-2-methyl-α-oxo-5-indanacetic acid methyl ester in 100 cc of methanol and 10 cc of concentrated sulphuric acid is hydrogenated at 45° and a hydrogen pressure of 5 atmospheres with the addition of 1.0 g of platinum(IV) oxide. After the take up of the theoretic amount of hydrogen the catalyst is filtered off, the solution is diluted with a 5% sodium bicarbonate solution and extracted with ether. The extract is washed with water, dried over sodium sulphate and concentrated by evaporation. The resulting title compound is purified by chromatography. Thin layer chromatogram: Rf value 0.60 (adsorbent: silica gel, eluant: chloroform).

Quelle