HRID2221760

反应详情

EQUATION

反应方程式

HRID 2221760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of ethyl 1-benzyl-3-[(4-{[2-(2-furyl)-5-methyl-1,3-oxazol-4-yl]methoxy}-3-(methoxymethoxy)benzyl)oxy]-1H-pyrazole-4-carboxylate (8.65 g), 1N hydrochloric acid (50 mL), tetrahydrofuran (100 mL) and ethanol (100 mL) was stirred at 50° C. for 5 hrs. The reaction mixture was diluted with ethyl acetate, and washed successively with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate-hexane (2:3, v/v) to give ethyl 1-benzyl-3-[(4-{[2-(2-furyl)-5-methyl-1,3-oxazol-4-yl]methoxy}-3-hydroxybenzyl)oxy]-1H-pyrazole-4-carboxylate as colorless crystals (5.37 g, yield 67%). Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 134-135° C.

WORKUP

后处理

  1. washwashed successively with water and saturated brine
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated
  4. washeluted with ethyl acetate-hexane (2:3