反応 #77837

反応方程式

triethylamine

ethyl isocyanate

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

HCl

→

benzamide

収率 17.5%

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

収率 17.5%

溶媒

THF

EtOAc

反応条件

後処理

1. 1
   洗浄The EtOAc layer was washed with 1 N HCl and brine
2. 2
   乾燥The EtOAc was dried (MgSO4)
3. 3
   ろ過filtered
4. 4
   濃縮concentrated
5. 5
   その他Reverse phase HPLC purification (gradient elution, water/acetonitrile/TFA)

実験手順

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.

出典