HRID1771604
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe THF removed in vacuo
- additionthe aqueous residue adjusted to pH 4 by addition of 1M HCl
- filtrationThe precipitate was collected by filtration
- customdried in vacuo
- customcrystallized from CH2Cl2 and petroleum ether