HRID507939

反应详情

EQUATION

反应方程式

HRID 507939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution (10 mL) of ethyl 5-isobutoxy-1-(2-methylphenyl)-1H-pyrazole-3-carboxylate (1.07 g, 3.54 mmol) in anhydrous tetrahydrofuran was added lithium aluminum hydride (0.13 g, 3.54 mmol) under stirring at 0° C., and the mixture was stirred at the same temperature for 2 hr. After completion of the reaction, sodium sulfate decahydrate (2.28 g, 7.08 mmol) was added to the reaction system and the mixture was stirred at room temperature for 2 hr. The precipitated insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1-1/1) to give the title compound (0.85 g, yield 92%) as a pale-yellow oil.

WORKUP

后处理

  1. stirringthe mixture was stirred at the same temperature for 2 hr
  2. additionwas added to the reaction system
  3. stirringthe mixture was stirred at room temperature for 2 hr
  4. filtrationThe precipitated insoluble material was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1-1/1)