HRID1790299
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
To a solution of 1-(1,4-dimethoxynaphthalen-2-yl)-propane-1,2-dione 2-oxime (1 g, 3.66 mmol, Example 2, Step B) in 1 M hydrogen chloride in ethanol (50 mL) was added Pd/C 10% (100 mg), The mixture was hydrogenated on a Parr hydrogenator apparatus under 40–50 psi pressure for 12 h. The catalyst was separated by filtration and the solvent removed in vacuo to give a white solid: 1H NMR (DMSO-d) δ 1.14 (d, 3H, CH3), 3.96 (s, 3H, OH3), 4.01 (s, 3H, OCH3), 5.03 (m, 1H, CH), 7.08 (s, 1H, Ar—H), 7.73 (m, 2H, Ar—H), 8.19 (m, 2H, Ar), 8.50 (bs, 3H, NH3+); Analysis calcd. for C15H17NO3.HCl.0.2 H2O: C, 53.62; H, 5.88; N, 4.81. Found: C, 53.53; H, 5.56; N, 4.77.
WORKUP
后处理
- customThe catalyst was separated by filtration
- customthe solvent removed in vacuo
- customto give a white solid