반응 #77837

반응 방정식

triethylamine

ethyl isocyanate

2-(amino)-N-[2-[[(cis)-2-[[4-(methylthio)benzoyl]amino]cyclohexyl]amino]-2-oxoethyl]-5-trifluoromethyl benzamide

HCl

→

benzamide

수율 17.5%

2-((Ethylaminocarbonyl)amino)-N-[2-[[(cis)-2-[[4-(methylthio)benzoyl]amino]cyclohexyl]amino]-2-oxoethyl]-5-trifluoromethyl benzamide

수율 17.5%

용매

THF

EtOAc

반응 조건

후처리

1. 1
   세척The EtOAc layer was washed with 1 N HCl and brine
2. 2
   건조The EtOAc was dried (MgSO4)
3. 3
   여과filtered
4. 4
   농축concentrated
5. 5
   기타Reverse phase HPLC purification (gradient elution, water/acetonitrile/TFA)

실험 절차

2-(amino)-N-[2-[[(cis)-2-[[4-(methylthio)benzoyl]amino]cyclohexyl]amino]-2-oxoethyl]-5-trifluoromethyl benzamide (Example 114a) (50 mg) was dissolved in THF (2.5 mL) prior to the addition of triethylamine (30 mg) and ethyl isocyanate (21 mg). After stirring for 72 h, EtOAc was added along with 1 N HCl solution. The EtOAc layer was washed with 1 N HCl and brine. The EtOAc was dried (MgSO4), filtered, and concentrated. Reverse phase HPLC purification (gradient elution, water/acetonitrile/TFA) provided the title benzamide (10 mg). MS found: (M+Na)+=602.4.

출처