HRID350448
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 stirred solution of methyl 3-bromo-4-[N′-(2-methylphenyl)ureido]phenylacetate (650 mg, 1.72 mmol) in THF (10 ml) was added 0.25 N NaOH (10 ml). After stirring at room temperature for 14 h, the solvent was concentrated in vacuo. The residue was triturated by the addition of 1 N HCl and dried at 60° C. for 2 days under a reduced pressure to give 3-bromo-4-[N′-(2-methylphenyl)ureido]phenylacetic acid (1.22 g, 100%) as colorless powder. 1H-NMR (DMSO-d6) δ 2.26 (s, 3H), 3.32 (s, 2H), 6.93 (m, 2H), 7.10–7.17 (m, 4H), 7.76 (d, J=8.1 Hz, 2H), 8.52 (s, 1H); MS (ESI) m/z 385 (M++Na), 387 (M++2+Na).
WORKUP
后处理
- concentrationthe solvent was concentrated in vacuo
- customThe residue was triturated by the addition of 1 N HCl
- customdried at 60° C. for 2 days under a reduced pressure