Reaktion #416787

Reaktionsgleichung

chloroformic acid vinyl ester

4-(4-(1,1-Dimethylethyl)-2-thiazolyl)-1-phenylmethyl-piperidine

K2CO3

→

title compound

4-(4-(1,1-Dimethylethyl)-2-thiazolyl)-piperidine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated
2. 2
   SonstigeThe residue is partitioned between ethyl ether and water
3. 3
   SonstigeThe ether phase is evaporated
4. 4
   workup.DISSOLUTIONthe residue dissolved in 30 ml metnanol and 30 ml 20% aqueous hydrochloric acid
5. 5
   TemperaturThe mixture is heated 1 hour at 60
6. 6
   Sonstigeevaporated
7. 7
   SonstigeThe residue is partitioned between aqueous NaOH and ether
8. 8
   workup.ADDITIONThe etner phase is treated with maleic acid

Vorschrift

4.8 g 4-(4-(1,1-Dimethylethyl)-2-thiazolyl)-1-phenylmethyl-piperidine, 2 g K2CO3 and 50 ml 1,2-dicnloroethane are treated dropwise at -5° under stirring with 3.2 g chloroformic acid vinyl ester. The mixture is stirred 2 hours at room temperature and evaporated. The residue is partitioned between ethyl ether and water. The ether phase is evaporated and the residue dissolved in 30 ml metnanol and 30 ml 20% aqueous hydrochloric acid. The mixture is heated 1 hour at 60 and evaporated. The residue is partitioned between aqueous NaOH and ether. The etner phase is treated with maleic acid to yield the hydrogenmaleinate of the title compound, m.p. 141°-142° (ethanol/ether).

Quelle