反応 #77835

反応方程式

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

3-chlorobenzenesulfonyl chloride

EtOAc

→

benzamide

収率 29.4%

4-(Aminosulfonyl)-N-{(cis)-2-[({[(3-chlorophenyl)sulfonyl]amino}acetyl)amino]cyclohexyl}benzamide

収率 29.4%

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), (70 mg) was dissolved in DMF (2.5 mL) prior to the addition of 3-chlorobenzenesulfonyl chloride (51 mg). 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 (25 mg). MS found: (M+H)+=530.1.

出典