HRID1771604

反应详情

EQUATION

反应方程式

HRID 1771604 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 isopropyl 2-[2,4-difluoro-3-[[3-(3-fluorophenyl)-5-methylphenyl]methylamino]phenoxy]acetate (127 mg, 0.29 mmol, 1.0 eq) in THF (3 mL) was added NaOH (2M aqueous solution, 0.57 mL, 1.15 mmol, 4.0 eq) at room temperature. The reaction was stirred at room temperature for 1 h and then the THF removed in vacuo and the aqueous residue adjusted to pH 4 by addition of 1M HCl. The precipitate was collected by filtration, dried in vacuo and crystallized from CH2Cl2 and petroleum ether to give the title compound (I(d)) as a white solid (50 mg, 44%).

WORKUP

后处理

  1. customthe THF removed in vacuo
  2. additionthe aqueous residue adjusted to pH 4 by addition of 1M HCl
  3. filtrationThe precipitate was collected by filtration
  4. customdried in vacuo
  5. customcrystallized from CH2Cl2 and petroleum ether