HRID2277407

反应详情

EQUATION

反应方程式

HRID 2277407 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

To a solution of N-(4-((7-hydroxy-6-methoxyquinolin-4-yl)oxy)phenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide (4.93 g, 9.93 mmol) and isobutylene oxide (8.8 mL, 100 mmol) in DMF/H2O (21 mL/4 mL) was added K2CO3 (2.74 g, 2 mmol). The reaction mixture was stirred at 60° C. for 12 hours, then cooled to room temperature and treated with aqueous NaH2PO4 (saturated solution, 10 mL) to adjust the pH of the mixture to 7˜8. The solid was collected by filtration and washed with EtOAc/EtOH (80 mL/15 mL). The title compound was obtained as a pale yellow solid (1.93 g, 34.3%).

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationThe solid was collected by filtration
  3. washwashed with EtOAc/EtOH (80 mL/15 mL)