HRID1294187
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of methyl 3-(5-methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolecarboxylate (5.27 g) in tetrahydrofuran (100 ml) was slowly added diisobutylaluminum hydride (0.95 M hexane solution, 60 ml) at 0° C. and the mixture was stirred at 0° C. for 1 hr. Sodium sulfate 10 hydrate (17.01 g) was added to the reaction mixture and the mixture was further stirred at room temperature for 30 min. The insoluble materials were removed by filtration, and the filtrate was concentrated to give [3-(5-methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolyl]methanol (3.88 g, 80%) as colorless crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point: 84-85° C.
WORKUP
后处理
- customat 0° C.
- stirringthe mixture was further stirred at room temperature for 30 min
- customThe insoluble materials were removed by filtration
- concentrationthe filtrate was concentrated