Reaktion #1828436

Reaktionsgleichung

Sodium

sodium

2',4',6'-trimethylbutyrophenone

diethyl oxalate

→

oil

Ausbeute 53.2%

Ethyl 3-ethyl-2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate

Ausbeute 53.2%

Lösungsmittel

EtOH

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirred overnight
2. 2
   SonstigeThe solvent was then evaporated
3. 3
   WaschenThe resulting residue was washed with hexane
4. 4
   workup.ADDITIONdiluted with water
5. 5
   Extraktionextracted with ether
6. 6
   WaschenThe extracts were washed with brine
7. 7
   Trocknendried over Na2SO4
8. 8
   Einengenconcentrated

Vorschrift

Sodium (1.0 g, 42.1 mmol, spheres ) was cautiously added to 25 mL of absolute EtOH with stirring. After the sodium had dissolved, diethyl oxalate (6.0 g, 42.1 mmol) was added dropwise to the resulting solution at 0° C., followed by addition of a solution of 2',4',6'-trimethylbutyrophenone (8 g, 42.1 mmol) in 5 mL of absolute EtOH. The reaction mixture was slowly warmed to 50° C. and stirred overnight. The solvent was then evaporated. The resulting residue was washed with hexane, diluted with water, acidified with 1 N HCl, and then extracted with ether. The extracts were washed with brine, dried over Na2SO4 and concentrated to give 6.5 g of an oil which was used in the next reaction without further purification.

Quelle