HRID632517

反应详情

EQUATION

反应方程式

HRID 632517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To 1.0 g of 2-methyl-4-(2-pyridylmethoxy)benzoic acid methyl ester was added 8 mL of toluene under argon atmosphere. To the mixture cooled to −78° C., 8.7 mL of a solution of diisobutylaluminium hydride (1.0 mol/L) in toluene was added dropwise. The mixture was stirred at the same temperature for 6 hours and further stirred at −35° C. for 1 hour. To the reaction mixture, a saturated aqueous Rochelle salt solution was added, and the mixture was stirred at room temperature for 30 minutes. To this, 150 mL of diethyl ether was added, and the organic layer was separated. The obtained organic layer was dried over Na2SO4 and concentrated to give 0.83 g of the title compound (93% yield).

WORKUP

后处理

  1. stirringfurther stirred at −35° C. for 1 hour
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. customthe organic layer was separated
  4. dry with materialThe obtained organic layer was dried over Na2SO4
  5. concentrationconcentrated