반응 #10167

반응 방정식

Methyl 4′-{[({1-[(tert-butoxycarbonyl)amino]cyclopropyl}carbonyl)-amino]methyl}-1,1′-biphenyl-2-carboxylate

hydrogen chloride

→

methyl 4′-({[(1-aminocyclopropyl)carbonyl]amino}methyl)-1,1′-biphenyl-2-carboxylate

용매

DCM

MeOH

chloroform

DCM

반응 조건

후처리

1. 1
   기타Dry nitrogen was then bubbled through the solution for about 30 min
2. 2
   기타Solvent was then removed under reduced pressure
3. 3
   기타to yield an oily residue
4. 4
   기타the solvent removed
5. 5
   기타was obtained
6. 6
   여과followed by saturation with ammonia gas, filtration and solvent removal

실험 절차

Methyl 4′-{[({1-[(tert-butoxycarbonyl)amino]cyclopropyl}carbonyl)-amino]methyl}-1,1′-biphenyl-2-carboxylate (0.84 g, 2.0 mmol) dissolved in a mixture of DCM (3 mL) and MeOH (45 mL) was cooled to 0° C. This homogenous solution was saturated with anhydrous hydrogen chloride and allowed to sit for 30 minutes. Dry nitrogen was then bubbled through the solution for about 30 min. Solvent was then removed under reduced pressure to yield an oily residue. The oil was then dissolved in DCM and the solvent removed. This process being repeated until a solid amine hydrochloride was obtained. Alternatively, the residue could be dissolved in chloroform followed by saturation with ammonia gas, filtration and solvent removal to obtain solid methyl 4′-({[(1-aminocyclopropyl)carbonyl]amino}methyl)-1,1′-biphenyl-2-carboxylate as the free-base.

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