HRID354367

反应详情

EQUATION

反应方程式

HRID 354367 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of ethyl 4-[N′-(2-methoxyphenyl)ureido]phenylacetate (2.22 g, 6.78 mmol) in MeOH (30 ml) was added 1.0 M-NaOH aq. (10.2 ml, 10.2 mmol), and the resulting mixture was stirred overnight 1N-HCl (aq.) was added and the mixture was concentrated in vacuo. Water was added to the residue to give precipitate, which was collected by filtration. The crude solid was recrystallized from EtOH/hexane to give 4-[N′-(2-methoxyphenyl)ureido]phenylacetic acid as a white powder (1.87 g, 92%). mp 165-168° C.; 1H-NMR (CD3OD) δ2.30 (s, 3 H), 3.55 (s, 2 H), 4.87 (s, 3 H), 6.87-6.92 (m, 2 H), 6.97-6.99 (m, 2 H), 7.10-7.24 (m, 2 H), 7.53-7.58 (m, 1 H), 8.04 (d, J=7.2 Hz, 1 H); MS (ESI) m/z 300 (M+).

WORKUP

后处理

  1. additionwas added
  2. concentrationthe mixture was concentrated in vacuo
  3. additionWater was added to the residue
  4. customto give precipitate, which
  5. filtrationwas collected by filtration
  6. customThe crude solid was recrystallized from EtOH/hexane