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
A mixture of ethyl (4-{4-[(4-[({4-[(E)-2-(1-ethyl-1H-imidazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]-2-methoxyphenoxy)methyl]-5-methyl-1,3-oxazol-2-yl)phenyl)acetate (485 mg), 8N aqueous sodium hydroxide solution (1 mL), tetrahydrofuran (5 mL) and ethanol (5 mL) was heated under reflux for 30 min. After cooling, to the reaction mixture was added 1N hydrochloric acid (8 mL) and the mixture was left standing overnight. The precipitated crystals were collected by filtration and recrystallized from methanol-diethyl ether to give (4-{4-[(4-[({4-[(E)-2-(1-ethyl-1H-imidazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]-2-methoxyphenoxy)methyl]-5-methyl-1,3-oxazol-2-yl}phenyl)acetic acid as colorless crystals (472 mg, yield 100%). melting point: 194-196° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 30 min
- temperatureAfter cooling, to the reaction mixture
- waitthe mixture was left
- filtrationThe precipitated crystals were collected by filtration
- customrecrystallized from methanol-diethyl ether