Reaktion #962475

Reaktionsgleichung

ethyl 2-hydroxycaproate

sodium methylate

methanol

orthophosphoric acid

dimethylamine

methanol

→

2-hydroxy-N,N-dimethylhexanamide

Ausbeute 81.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis brought to 40° C.
2. 2
   Temperaturmaintained for 3 hours
3. 3
   Sonstigeis obtained
4. 4
   SonstigeThe salts formed
5. 5
   Sonstigeare removed by filtration
6. 6
   Sonstigethe solvents are removed under reduced pressure

Vorschrift

In a three-neck flask, at 20° C. and under an inert atmosphere, are mixed ethyl 2-hydroxycaproate (24.24 g; 150 mmol) and sodium methylate in solution in methanol (25% w/w) (1.6 g; 7 mmol). To this mixture, is added dimethylamine in solution in methanol (50% w/w) (26.75 g; 297 mmol) within 30 minutes. The temperature of this mixture is brought to 40° C. and maintained for 3 hours. After the return of the temperature of this reaction mixture to 20° C., orthophosphoric acid is added until a pH of 5 is obtained. The salts formed are removed by filtration and the solvents are removed under reduced pressure. 2-hydroxy-N,N-dimethylhexanamide is then obtained with a purity of 98%, i.e. a yield of 81%.

Quelle