Reaktion #44973

Reaktionsgleichung

hydrochloric acid

Methyl trans-4-aminocyclohexanecarboxylate hydrochloride

triethylamine

2-chloroethyl chloroformate

→

methyl trans-4-{[(2-chloroethoxy)carbonyl]amino}cyclohexanecarboxylate

Lösungsmittel

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling
2. 2
   Extraktionthe mixture is extracted with chloroform
3. 3
   WaschenThe organic layer is washed with saturated brine
4. 4
   Trocknendried over sodium sulfate
5. 5
   Sonstigeevaporated
6. 6
   Sonstigeto remove the solvent under reduced pressure
7. 7
   FiltrationThe precipitates are collected by filtration
8. 8
   Sonstigedried

Vorschrift

Methyl trans-4-aminocyclohexanecarboxylate hydrochloride (5.00 g) obtained in Reference Example 2(1) is dissolved in chloroform (60 ml), and thereto is added triethylamine (11 ml) under ice-cooling, followed by dropwise addition of a solution of 2-chloroethyl chloroformate (3.3 ml) in chloroform (10 ml). After stirring at room temperature for 2.5 hours, to the reaction solution is added 5% hydrochloric acid and the mixture is extracted with chloroform. The organic layer is washed with saturated brine, dried over sodium sulfate, and then evaporated to remove the solvent under reduced pressure. The resulting residue is suspended in chloroform/diisopropyl ether. The precipitates are collected by filtration and dried to give methyl trans-4-{[(2-chloroethoxy)carbonyl]amino}cyclohexanecarboxylate (5.11 g).

Quelle