反応 #1702119

反応方程式

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

methanol

acetic acid

NaHCO3

→

desired product

収率 97.0%

3-Amino-N-(3-{[(2,5-dichloropyrimidin-4-yl)amino]methyl}phenyl)benzamide

収率 97.0%

溶媒

water

EtOAc

反応条件

後処理

1. 1
   温度After cooling
2. 2
   ろ過the mixture was filtered
3. 3
   洗浄washed with EtOAc
4. 4
   濃縮The filtrate was concentrated under vacuum
5. 5
   その他to give a residue, which
6. 6
   その他The organic layer was dried
7. 7
   濃縮concentrated under vacuum

実験手順

Into a reaction flask were added N-(3-{[(2,5-dichloropyrimidin-4-yl)amino]methyl}phenyl)-3-nitrobenzamide (0.30 g, 0.72 mmol), methanol (20 mL), acetic acid (2.0 mL), and water (1 mL). Then iron (0.50 g, 9.0 mmol) powder was added. The reaction mixture was heated at 70° C. overnight. After cooling, the mixture was filtered and washed with EtOAc. The filtrate was concentrated under vacuum to give a residue, which was treated with NaHCO3 (saturated aqueous solution) and EtOAc. The organic layer was dried and concentrated under vacuum to provide the desired product (0.27 g, 97%). LCMS for C18H16Cl2N5O (M+H)+: m/z=388.0, 390.0.

出典