HRID2221969

反应详情

EQUATION

反应方程式

HRID 2221969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 3-{[3-methoxy-4-(5-methyl-2-phenyl-1,3-oxazol-4-ylmethoxy)benzyl]oxy}-1-phenyl-1H-pyrazole-5-carboxylate (6.00 g) in tetrahydrofuran (20 mL) was slowly added lithium aluminum hydride (400 mg) at 0° C., and the mixture was stirred for 30 min. Sodium sulfate decahydrate (4.16 g) was added to the reaction mixture, the precipitate was filtered off, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography to give (3-{[3-methoxy-4-(5-methyl-2-phenyl-1,3-oxazol-4-ylmethoxy)benzyl]oxy}-1-phenyl-1H-pyrazol-5-yl)methanol (5.19 g, yield 92%) as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:1, v/v). The crystals were recrystallized from ethyl acetate-hexane. melting point: 146-147° C.

WORKUP

后处理

  1. customat 0° C.
  2. filtrationthe precipitate was filtered off
  3. concentrationthe filtrate was concentrated