HRID448433

反应详情

EQUATION

反应方程式

HRID 448433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium hydroxide (0.4 g, 10.5 mmol) in water (10 mL) was added to a stirred suspension of 3-ureidomethyl-phthalic acid dimethyl ester (1.4 g, 5.3 mmol) in ethanol (30 mL). The mixture was refluxed for one hour and then cooled to room temperature. The mixture was concentrated, and the residue was dissolved in water (30 mL). The mixture was acidified with 4N HCl to pH 1. The mixture was filtered to give 3-ureidomethyl-phthalic acid (1.0 g, 76%): 1H NMR (DMSO-d6) δ 4.22 (d, J=5.9 Hz, 2H, CH2), 5.68 (s, 2H, NH2), 6.40 (t, J=6.0 Hz, 1H, NH), 7.46-7.56 (m, 2H, Ar), 7.73 (d, J=6.9 Hz, 1H, Ar), 13.23 (b, 2H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for one hour
  2. concentrationThe mixture was concentrated
  3. dissolutionthe residue was dissolved in water (30 mL)
  4. filtrationThe mixture was filtered