反応 #1702116

反応方程式

N-(3-aminobenzyl)-2,5-dichloropyrimidin-4-amine

hydrogen chloride

triethylamine

m-nitrobenzenesulfonyl chloride

→

desired product

収率 95.0%

N-(3-{[(2,5-Dichloropyrimidin-4-yl)amino]methyl}phenyl)-3-nitrobenzenesulfonamide

収率 95.0%

溶媒

THF

反応条件

後処理

1. 1
   その他the solvent was removed under vacuum
2. 2
   workup.ADDITIONThe residue was treated with EtOAc and water
3. 3
   乾燥The organic layer was dried over Na2SO4
4. 4
   ろ過filtered
5. 5
   濃縮concentrated under vacuum

実験手順

To a mixture of N-(3-aminobenzyl)-2,5-dichloropyrimidin-4-amine.hydrogen chloride (0.20 g, 0.58 mmol) and triethylamine (0.32 mL, 2.3 mmol) in THF (3 mL) was added slowly m-nitrobenzenesulfonyl chloride (0.13 g, 0.58 mmol). The resulting mixture was stirred at rt for 2 hours and the solvent was removed under vacuum. The residue was treated with EtOAc and water. The organic layer was dried over Na2SO4, filtered, and concentrated under vacuum to provide the desired product (0.30 g, 95%). LCMS for C17H14Cl2N5O4S (M+H)+: m/z=453.9, 455.9.

出典