反应 #2320166

反应方程式

solution

N-{[2-(1,4-diazepan-1-yl)pyridin-3-yl]methyl}-4-(2,3-dichlorophenyl)-4H-1,2,4-triazol-3-amine

potassium carbonate

bromoacetamide

→

title compound

收率 38.4%

2-[4-(3-{[4-(2,3-Dichloro-phenyl)-4H-[1,2,4]triazol-3-ylamino]-methyl}-pyridin-2-yl)-[1,4]diazepan-1-yl]-acetamide

收率 38.4%

溶剂

dimethylformamide

反应条件

后处理

1. 1
   workup.ADDITIONthen poured onto ice water
2. 2
   萃取The aqueous mixture was extracted with dichloromethane
3. 3
   洗涤The organic layer was washed with brine
4. 4
   干燥dried over magnesium sulfate
5. 5
   过滤filtered
6. 6
   浓缩concentrated
7. 7
   其他The residue was purified by flash column chromatography

实验过程

To a solution of Example 113A (250 mg, 0.597 mmol) in dimethylformamide (7 ml) was added potassium carbonate (165 mg, 1.194 mmol) and bromoacetamide (124 mg, 0.896 mmol). The reaction mixture was stirred at room temperature for 16 hours then poured onto ice water. The aqueous mixture was extracted with dichloromethane. The organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated. The residue was purified by flash column chromatography using dichloromethane/methanol (80:20) to give the title compound (109 mg). MS (ESI+) m/z 475.6 (M+H)+; Rt=1.41. 1H NMR (DMSO-d6) δ 8,170 (s, 1H); 8,054 (d,1H); 7,832 (d,1H); 7,579(m,3H); 7,251 (s,1H); 7,112 (s,1H); 6,832 (dd,1H); 6,545 (t,1H); 4,338 (d, 2H); 3,423 (m,4H); 3,011 (s,2H); 2,772 (m,2H); 2,710 (m,2H); 1,856(m,2H).

来源