反应详情

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 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.

1. temperaturethe mixture is heated
2. temperatureto reflux with a water trap for one hour
3. temperatureThe mixture is then cooled
4. customthe phases are separated
5. extractionThe aqueous phase is then extracted again
6. stirringby shaking with chloroform
7. dry with materialthe organic phase is dried over sodium sulphate
8. filtrationfiltered
9. customevaporated to dryness
10. dissolutionThe resulting residue is dissolved in ether
11. additionethereal hydrochloric acid is added
12. customthe mixture is evaporated to dryness
13. customthe residue is triturated with acetone
14. filtrationfiltered off with suction