反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of N-(4-((6-nitropyridin-3-yl)oxy)pyridin-2-yl)cyclopropanecarboxamide (1.50 g, 5.00 mmol) in MeOH (30 mL) was treated with hydrazine hydrate (1.50 g, 30.0 mmol) followed by Raney nickel (0.300 g, 5.11 mmol) and stirred at RT for 3 h. The solids were removed via filtration through diatomaceous earth, rinsed with DCM, then MeOH and the filtrate concentrated to dryness to afford N-(4-((6-aminopyridin-3-yl)oxy)pyridin-2-yl)cyclopropanecarboxamide (1.17 g, 87%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 11.21 (s, 1H), 8.56 (d, J=5.7 Hz, 1H), 8.19 (s, 1H), 8.01 (s, 1H), 7.68 (d, J=8.9 Hz, 1H), 7.06 (m, 1H), 6.92 (d, J=8.9 Hz, 1H), 6.43 (s, 2H), 2.37 (m, 1H), 1.18 (s, 4H); MS (ESI) m/z: 271.2 (M+H+).
WORKUP
后处理
- customThe solids were removed via filtration through diatomaceous earth
- washrinsed with DCM
- concentrationMeOH and the filtrate concentrated to dryness