HRID626522
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 mixture of 1,1-dimethyl-3-(4-((2-methyl-6-nitropyridin-3-yl)oxy)pyridin-2-yl)urea (0.500 g, 1.576 mmol) and NH4Cl (2.53 g, 47.3 mmol) in MeOH (10 mL) and THF (10 mL) was treated with zinc dust (1.030 g, 15.76 mmol) and stirred at RT for 0.5 h. The mixture was diluted with EtOAc, the solids removed via filtration, washed with EtOAc and the filtrate concentrated to dryness. The residue was treated with DCM, sonicated, the solids removed via filtration and the filtrate concentrated to dryness to afford 3-(4-((6-amino-2-methylpyridin-3-yl)oxy)pyridin-2-yl)-1,1-dimethylurea (510 mg, 113%). MS (ESI) m/z: 288.1 (M+H+).
WORKUP
后处理
- customthe solids removed via filtration
- washwashed with EtOAc
- concentrationthe filtrate concentrated to dryness
- additionThe residue was treated with DCM
- customsonicated
- customthe solids removed via filtration
- concentrationthe filtrate concentrated to dryness