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 3-[(4-{[2-(2-furyl)-5-methyl-1,3-oxazol-4-yl]methoxy}-3-methoxybenzyl)oxy]-1-methyl-1H-pyrazole-4-carboxylate (7.54 g) in tetrahydrofuran (100 mL) was added lithium aluminum hydride (0.61 g) at 0° C. and the mixture was stirred at room temperature for 1 hr. Sodium sulfate decahydrate (5.19 g) was added to the reaction mixture and the mixture was stirred at room temperature for 30 min. The reaction mixture was diluted with ethyl acetate and the precipitate was filtered off, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography to give {3-[(4-{[2-(2-furyl)-5-methyl-1,3-oxazol-4-yl]methoxy}-3-methoxybenzyl)oxy]-1-methyl-1H-pyrazol-4-yl}methanol as colorless crystals (4.15 g, yield 61%) from a fraction eluted with ethyl acetate-hexane (5:1, v/v). Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 132-133° C.
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 30 min
- filtrationthe precipitate was filtered off
- concentrationthe filtrate was concentrated