HRID486939

反应详情

EQUATION

反应方程式

HRID 486939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

32 ml of a 1.4M solution of methyllithium in diethyl ether was dissolved in 50 ml of anhydrous tetrahydrofuran. The obtained solution was cooled to -40° C. in a nitrogen atmosphere, followed by the addition of 5.0 g of solid (6-methyl-1,3-benzodioxol-5-yl)carboxaldehyde. The mixture was heated to a room temperature over a period of one hour, followed by the addition of water. The obtained mixture was extracted with ether and the obtained organic layer was washed with an aqueous solution of common salt, dried over magnesium sulfate and distilled to remove the solvent. The obtained white solid was recrystallized from diisopropyl ether/n-hexane to obtain 2.8 g of the title compound as a colorless crystal.

WORKUP

后处理

  1. temperatureThe mixture was heated to a room temperature over a period of one hour
  2. extractionThe obtained mixture was extracted with ether
  3. washthe obtained organic layer was washed with an aqueous solution of common salt
  4. dry with materialdried over magnesium sulfate
  5. distillationdistilled
  6. customto remove the solvent
  7. customThe obtained white solid was recrystallized from diisopropyl ether/n-hexane