HRID1294191

反应详情

EQUATION

反应方程式

HRID 1294191 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 ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate (15.00 g) in tetrahydrofuran (150 mL) was added lithium aluminum hydride (1.93 g) at 0° C., and the mixture was stirred at room temperature for 1 hr. Sodium sulfate 10 hydrate (21.03 g) and hexane (100 mL) were added to the reaction mixture, and the mixture was stirred at room temperature for 1 hr. The precipitate was removed by filtration and the filtrate was concentrated. The obtained crystals were collected by filtration to give [3-methyl-1-(2-pyridyl)-1H-pyrazol-4-yl]methanol (11.38 g). The crystals were recrystallized from acetone-hexane. melting point: 116-117° C.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 1 hr
  2. customThe precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. filtrationThe obtained crystals were collected by filtration