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 mixture of methyl 3-[4-({2-methoxy-4-[({4-[(E)-2-(5-methyl-2-morpholin-4-yl-1,3-thiazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]phenoxy}methyl)-5-methyl-1,3-oxazol-2-yl]benzoate (0.35 g), tetrahydrofuran (50 mL) and methanol (20 mL) was added 1N aqueous sodium hydroxide solution (20 mL), and the mixture was heated under reflux for 2 hrs. 1N Hydrochloric acid and water were added to acidify the reaction mixture, and the precipitated crystals were collected by filtration and washed with diethyl ether to give 3-[4-({2-methoxy-4-[({4-[(E)-2-(5-methyl-2-morpholin-4-yl-1,3-thiazol-4-yl)ethenyl]-1-phenyl-1H-pyrazol-3-yl}oxy)methyl]phenoxy)methyl)-5-methyl-1,3-oxazol-2-yl]benzoic acid as brown crystals (0.25 g, yield 71%). Recrystallization from acetone-hexane gave brown prism crystals. melting point: 215-217 (dec) ° C.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 2 hrs
- filtrationthe precipitated crystals were collected by filtration
- washwashed with diethyl ether