반응 #44973

반응 방정식

hydrochloric acid

Methyl trans-4-aminocyclohexanecarboxylate hydrochloride

triethylamine

2-chloroethyl chloroformate

→

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

용매

chloroform

chloroform

반응 조건

후처리

1. 1
   온도cooling
2. 2
   추출the mixture is extracted with chloroform
3. 3
   세척The organic layer is washed with saturated brine
4. 4
   건조dried over sodium sulfate
5. 5
   기타evaporated
6. 6
   기타to remove the solvent under reduced pressure
7. 7
   여과The precipitates are collected by filtration
8. 8
   기타dried

실험 절차

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).

출처