反応 #77834

反応方程式

EtOAc

4-methylmorpholine

2-trifluoromethylphenyl isocyanate

N-(cis)-{2-[(aminoacetyl)amino]cyclohexyl}-4-(aminosulfonyl)benzamide hydrogen bromide

→

benzamide

4-(Aminosulfonyl)-N-((cis)-2-{[({[2-(trifluoromethyl)anilino]carbonyl}amino)acetyl]amino}cyclohexyl)benzamide

溶媒

DMF

反応条件

後処理

1. 1
   洗浄the solution was washed with 1N HCl
2. 2
   乾燥The EtOAc was dried
3. 3
   ろ過filtered
4. 4
   濃縮concentrated
5. 5
   その他Reverse phase HPLC purification (gradient elution, water/acetonitrile/TFA) of the resulting residue

実験手順

N-(cis)-{2-[(aminoacetyl)amino]cyclohexyl}-4-(aminosulfonyl)benzamide hydrogen bromide, (61b), (100 mg) was dissolved in DMF (3 mL) prior to the addition of 4-methylmorpholine (0.13 mL) and 2-trifluoromethylphenyl isocyanate (0.05 mL). After stirring overnight, EtOAc was added and the solution was washed with 1N HCl. The EtOAc was dried, filtered, and concentrated. Reverse phase HPLC purification (gradient elution, water/acetonitrile/TFA) of the resulting residue provided the title benzamide (50 mg). MS found: (M+Na)+=564.3.

出典