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 5-(5-methyl-2-phenyl-4-oxazolyl)methoxy-3-pyridinecarboxylate (10.70 g) and tetrahydrofuran (100 mL) was added lithium aluminum hydride (1.02 g) under ice-cooling, and the mixture was stirred at room temperature for 10 min. To the mixture was added sodium sulfate 10 hydrate (8.38 g), and the mixture was further stirred at room temperature for 30 min. The insoluble materials were removed by filtration, and the filtrate was concentrated. The obtained residue was subjected to silica gel column chromatography to give crystals (8.93 g, 91%) of [5-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridyl]methanol from a fraction eluted with ethyl acetate-hexane (1:1, v/v). Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 111-112° C.
WORKUP
后处理
- temperaturecooling
- stirringthe mixture was further stirred at room temperature for 30 min
- customThe insoluble materials were removed by filtration
- concentrationthe filtrate was concentrated