Reaktion #73585

Reaktionsgleichung

N-(2-fluoroethyl)-N-methylaminooxamic acid

methanol

sodium hydroxide

hydrochloric acid

→

N-(2-fluoroethyl)-N-methyloxamic acid

Ausbeute 66.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling, to the suspension
2. 2
   Extraktionthe mixture was then extracted with ethyl acetate
3. 3
   Sonstigethe organic phase thus separated
4. 4
   Waschenwas washed with water
5. 5
   Trocknendried over magnesium sulfate
6. 6
   workup.DISTILLATIONthe ethyl acetate was distilled off from the organic phase
7. 7
   Sonstigeto thus give, as the target product, 0.94 g (yield: 66%

Vorschrift

To a mixed solvent comprising 6 ml of methanol and 5 ml of water, there was suspended 1.56 g of N-(2-fluoroethyl)-N-methylmethoxyoxalylamide, then 3.2 g of a 15% aqueous solution of sodium hydroxide was dropwise added, with ice-cooling, to the suspension and then the mixture was stirred for one hour. Concentrated hydrochloric acid was added to the reaction system, the mixture was then extracted with ethyl acetate, the organic phase thus separated was washed with water, dried over magnesium sulfate and then the ethyl acetate was distilled off from the organic phase to thus give, as the target product, 0.94 g (yield: 66%, a solid product) of N-(2-fluoroethyl)-N-methylaminooxamic acid.

Quelle