反応 #1702118

反応方程式

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

hydrogen chloride

triethylamine

3-nitrobenzoyl chloride

→

desired product

収率 70.0%

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

収率 70.0%

溶媒

THF

反応条件

後処理

1. 1
   濃縮concentrated under vacuum
2. 2
   その他The residue was partitioned in EtOAc
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 (0.10 g, 0.29 mmol) (prepared according to Example 3, step B) and triethylamine (0.16 mL, 1.2 mmol) in THF (3 mL) was added slowly 3-nitrobenzoyl chloride (54 mg, 0.29 mmol). The resulting mixture was stirred at rt for 2 hours and concentrated under vacuum. The residue was partitioned in EtOAc and water. The organic layer was dried over Na2SO4, filtered, and concentrated under vacuum to give the desired product as a yellow solid (90 mg, 70%). LCMS for C18H14Cl2N5O3 (M+H)+: m/z=418.0, 420.0.

出典