HRID1070686

反应详情

EQUATION

反应方程式

HRID 1070686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-hydroxyphthalic acid (0.91 mg, 5.0 mmol) and carbonyldiimidazole (0.85 g, 5 mmol) in N,N-dimethylacetamide (3 mL) was stirred at room temperature for 45 min. To this mixture was added 2-methoxyethylamine (0.47 g, 6.0 mmol) and the resulting mixture heated under reflux for 15 min. After cooling to room temperature, the mixture was evaporated and the residue was purified by chromatography (SiO2, CH2Cl2: 2N NH3/MeOH 19:1 to 9:1) to afford the title compound (1.1 g, 95%) as a light yellow solid. MS: m/e=220.1 (M−H−).

WORKUP

后处理

  1. temperaturethe resulting mixture heated
  2. temperatureunder reflux for 15 min
  3. temperatureAfter cooling to room temperature
  4. customthe mixture was evaporated
  5. customthe residue was purified by chromatography (SiO2, CH2Cl2: 2N NH3/MeOH 19:1 to 9:1)