반응 #1702119

반응 방정식

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

methanol

acetic acid

NaHCO3

→

desired product

수율 97.0%

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

수율 97.0%

용매

water

EtOAc

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   여과the mixture was filtered
3. 3
   세척washed with EtOAc
4. 4
   농축The filtrate was concentrated under vacuum
5. 5
   기타to give a residue, which
6. 6
   기타The organic layer was dried
7. 7
   농축concentrated under vacuum

실험 절차

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.

출처