Reaktion #564313

Reaktionsgleichung

ethanol

sulphuric acid

N-[2-(4-carboxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine

chloroform

ammonia

→

N-[2-(4-Carboethoxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine hydrochloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe the mixture is heated
2. 2
   Temperaturto reflux with a water trap for one hour
3. 3
   TemperaturThe mixture is then cooled
4. 4
   Sonstigethe phases are separated
5. 5
   ExtraktionThe aqueous phase is then extracted again
6. 6
   workup.STIRRINGby shaking with chloroform
7. 7
   Trocknenthe organic phase is dried over sodium sulphate
8. 8
   Filtrationfiltered
9. 9
   Sonstigeevaporated to dryness
10. 10
    workup.DISSOLUTIONThe resulting residue is dissolved in ether
11. 11
    workup.ADDITIONethereal hydrochloric acid is added
12. 12
    Sonstigethe mixture is evaporated to dryness
13. 13
    Sonstigethe residue is triturated with acetone
14. 14
    Filtrationfiltered off with suction

Vorschrift

0.5 g (0.0012 mol) of N-[2-(4-carboxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine is dissolved in 150 ml of chloroform and, while stirring, 2 ml ethanol and 0.25 g of concentrated sulphuric acid are added, and the the mixture is heated to reflux with a water trap for one hour. The mixture is then cooled, ice-water is added, the mixture is made alkaline with ammonia and the phases are separated. The aqueous phase is then extracted again by shaking with chloroform, and the organic phase is dried over sodium sulphate, filtered and evaporated to dryness. The resulting residue is dissolved in ether, ethereal hydrochloric acid is added, the mixture is evaporated to dryness, and the residue is triturated with acetone and filtered off with suction.

Quelle