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-chlorophenyl)ureido]phenylacetate (710 mg, 1.79 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-chlorophenyl) ureido]phenylacetic acid (643 mg, 94%) as colorless powder. 1H-NMR (DMSO-d6) δ 3.56 (s, 2H), 7.05 (m, 1H), 7.21 (dd, J=8.6, 1.7 Hz, 1H), 7.29 (t, J=7.8 Hz, 1H), 7.46 (d, J=8.1 Hz, 1H), 7.46 (d, J=8.1 Hz, 1H), 7.53 (d, J=1.7 Hz, 1H), 7.83 (d, J=8.3 Hz, 1H), 8.06 (d, J=7.6 Hz, 1H), 8.86 (s, 1H), 8.89 (s, 1H), 12.40 (s, 1H); MS (ESI) m/z 382 (M++1), 384(M++3).
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