HRID1771668
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 solution of ethyl 2-[2-chloro-4-fluoro-3-[[2-fluoro-5-(3-fluorophenyl)phenyl]methylamino]phenoxy]acetate (155 mg, 0.34 mmol) in THF (2 mL) was added LiOH (2M aqueous solution, 2.5 mL, 2.5 mmol, 7.4 eq). The reaction mixture was stirred at room temperature for 2 h, then the organic solvent was removed in vacuo. The residue that remained was diluted with water and adjusted to pH 4-6 by addition of diluted HCl. The solid precipitate that formed was collected by filtration, washed with water and dried in vacuo to afford a crude product which was crystallized from DCM (1 mL) and hexane (20 mL) to give the title compound (I(o)) as a white solid (100 mg, 69%).
WORKUP
后处理
- customthe organic solvent was removed in vacuo
- additionThe residue that remained was diluted with water
- additionadjusted to pH 4-6 by addition of diluted HCl
- customThe solid precipitate that formed
- filtrationwas collected by filtration
- washwashed with water
- customdried in vacuo
- customto afford a crude product which
- customwas crystallized from DCM (1 mL) and hexane (20 mL)