HRID853436

反应详情

EQUATION

反应方程式

HRID 853436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

After dissolving N-(4-(7-(benzyloxy)-6-cyano-4-quinolyl)oxyphenyl)-N′-(4-fluorophenyl)urea (6.20 g, 12.3 mmol) in trifluoroacetic acid (60 ml) and thioanisole (3.6 ml, 30.7 mmol) under a nitrogen atmosphere, the solution was stirred at 60° C. overnight. The reaction solution was concentrated under reduced pressure, and after adding water (100 ml) to the obtained residue, sodium bicarbonate was added to neutralization, diethylether (200 ml) was added, the mixture was stirred, and the precipitated crystals were filtered out, washed with water and diethyl ether and dried at 70° C. to obtain the title compound (4.816 g, 11.6 mmol, 94.8%) as yellow crystals.

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionafter adding water (100 ml) to the obtained residue, sodium bicarbonate
  3. additionwas added to neutralization, diethylether (200 ml)
  4. additionwas added
  5. stirringthe mixture was stirred
  6. filtrationthe precipitated crystals were filtered out
  7. washwashed with water and diethyl ether
  8. customdried at 70° C.