HRID1070411

反应详情

EQUATION

反应方程式

HRID 1070411 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of methyl-5-phenyl-2-aminobenzoate (0.40 g, 1.76 mmol) and pyridine (0.285 mL, 3.52 mmol) in toluene (7 mL) at room temperature under argon was added 20% phosgene in toluene (1.32 mL, 2.55 mmol) and the mixture was heated at 90° C. for 1 h. The mixture was filtered, and the filtrate was concentrated to dryness. The crude material was dissolved in toluene (10 mL), biphenyl-4-methanol (0.270 g, 1.46 mmol) and DMAP (0.018 g, 0.146 mmol) were added and the mixture was heated at 90° C. for 18 h. The solvent was evaporated to dryness to give 0.51 g of 4-(biphenyl-4-ylmethoxycarbonylamino)-biphenyl-3-carboxylic acid methyl ester.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated to dryness
  3. dissolutionThe crude material was dissolved in toluene (10 mL)
  4. temperaturethe mixture was heated at 90° C. for 18 h
  5. customThe solvent was evaporated to dryness