HRID1352810
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 diethyl 5-[[(phenylmethoxy)amino]carbonyl]-1,3-benzenedicarboxylate (0.742 g, 2.0 mmol) in ethanol (10 mL) was added a suspension of Pd/C in ethanol (5 mL), and the mixture was shaken under hydrogen (50 psi) for 20 hours. The catalyst was removed by filtration through a pad of celite and the filtrate was concentrated to give white powder. This material was washed with ethanol (10 mL×2) and dried under vacuum to give 0.380 g of white powder: 1H NMR (CD3OD) δ 1.44 (t, 6H), 4.45 (q, 4H), 8.60 (s, 2H), 8.72 (s, 1H). TLC: Rf 0.20 (EtOAc/Hexanes 1/1).
WORKUP
后处理
- customThe catalyst was removed by filtration through a pad of celite
- concentrationthe filtrate was concentrated
- customto give white powder
- washThis material was washed with ethanol (10 mL×2)
- customdried under vacuum