HRID1294118

反应详情

EQUATION

反应方程式

HRID 1294118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooling
  2. stirringthe mixture was further stirred at room temperature for 30 min
  3. customThe insoluble materials were removed by filtration
  4. concentrationthe filtrate was concentrated