反応 #574073

反応方程式

(6-methyl-1,3-benzodioxol-5-yl)carboxaldehyde

magnesium ribbon

bromoethane

ammonium chloride

→

intended compound

収率 95.9%

1-(6-Methyl-1,3-benzodioxol-5-yl)-1-propanol

収率 95.9%

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   workup.DISTILLATIONThe solvent was distilled off
2. 2
   抽出After extraction with ethyl acetate
3. 3
   乾燥by drying over magnesium sulfate and concentration under reduced pressure
4. 4
   その他the residue was purified

実験手順

A solution of 2.0 g of (6-methyl-1,3-benzodioxol-5-yl)carboxaldehyde in 15 ml of anhydrous tetrahydrofuran was added dropwise at room temperature to a Grignard reagent prepared from 0.32 g of magnesium ribbon, 20 ml of anhydrous tetrahydrofuran and 1.4 g of bromoethane. The mixture was stirred for 2 h. A saturated ammonium chloride solution was added to the reaction mixture. The solvent was distilled off. After extraction with ethyl acetate followed by drying over magnesium sulfate and concentration under reduced pressure, the residue was purified according to silica gel column chromatography (ethyl acetate/hexane=2:8) to obtain 2.27 g of the intended compound in the form of white crystals.

出典