反应 #2320167

反应方程式

sodium bicarbonate

solution

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

acetone

sodium triacetoxyborohydride

→

title compound

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

溶剂

1,2-dichloroethane

反应条件

后处理

1. 1
   其他the layers were separated
2. 2
   萃取The aqueous layer was extracted with dichloromethane
3. 3
   洗涤The combined 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 in 1,2-dichloroethane (10 ml) was added acetone (3 mL) and sodium triacetoxyborohydride (253 mg, 1.194 mmol). The reaction mixture was stirred at room temperature overnight. Saturated sodium bicarbonate was added and the layers were separated. The aqueous layer was extracted with dichloromethane. The combined 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. MS (ESI+) m/z 460.6 (M+H)+; Rt=1.47. 1H NMR (DMSO-d6) δ 8,171 (s, 1H); 8,049 (d, 1H); 7,831(d, 1H); 7,586(m, 3H); 6,837 (dd, 1H); 6,521 (t, 1H); 4,353 (d, 2H); 3,377 (m, 4H); 3,289 (m, 1H); 2,862 (m, 2H); 2,642 (m, 2H); 1,773 (m, 2H); 0,949 (m, 6H).

来源