HRID1525676

反应详情

EQUATION

反应方程式

HRID 1525676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of tert-butyl 5-chloro-4-(((5-chloro-6-cyclopropylpyridin-3-yl)oxy)methyl)-2-fluorobenzoate (Preparation 26, 1.24 g, 3.01 mmol) in dichloromethane (22 mL) was added TFA (10.0 mL, 0.02 mol). The mixture was stirred under nitrogen at room temperature for 18 hours. Additional TFA (2.50 mL, 32.0 mmol) was added and stirring continued for 3 hours. The reaction mixture was evaporated under reduced pressure and the resulting residue dissolved in EtOAc (25 mL) and washed with 2M aqueous solution of HCl (25 mL). The resulting solid was filtered to afford the title compound (1.4 g, crude quant.) which was used with no further purification.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 3 hours
  3. customThe reaction mixture was evaporated under reduced pressure
  4. dissolutionthe resulting residue dissolved in EtOAc (25 mL)
  5. washwashed with 2M aqueous solution of HCl (25 mL)
  6. filtrationThe resulting solid was filtered