HRID2216925

反应详情

EQUATION

反应方程式

HRID 2216925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of [2-(methoxycarbonyl-phenyl-amino)-phenyl]-acetic acid (16 g, 55.5 mmol) and polyphosphoric acid (29 g, 167 mmol in terms of P2O5) is heated to 100° C. for 4 hours. To the reaction mixture, water (41 ml) is added dropwise at 85–100° C. with stirring and cooling. At 65° C. toluene (41 ml) is added and the mixture is stirred for 30 min. The two phases are separated and washed. The organic phases are concentrated and allowed to crystallize at 0° C. to yield 12 g of pure title compound (80%).

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture is stirred for 30 min
  3. customThe two phases are separated
  4. washwashed
  5. concentrationThe organic phases are concentrated
  6. customto crystallize at 0° C.