反応 #574072

反応方程式

Water

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

methyllithium

→

intended compound

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

溶媒

diethyl ether

tetrahydrofuran

反応条件

後処理

1. 1
   抽出After extraction with ether
2. 2
   洗浄the organic layer was washed with an aqueous common salt solution
3. 3
   乾燥After drying over magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   その他to obtain a white solid, which
6. 6
   その他was recrystallized from diisopropyl ether/n-hexane

実験手順

32 ml of a 1.4M solution of methyllithium in diethyl ether was dissolved in 50 ml of anhydrous tetrahydrofuran and the solution was cooled at -40° C. in a nitrogen atmosphere. 5.0 g of solid (6-methyl-1,3-benzodioxol-5-yl) carboxaldehyde was added to the solution and the temperature was elevated to room temperature gradually over 1 h. Water was added to the reaction mixture. After extraction with ether, the organic layer was washed with an aqueous common salt solution. After drying over magnesium sulfate, the solvent was distilled off to obtain a white solid, which was recrystallized from diisopropyl ether/n-hexane to obtain 2.8 g of the intended compound in the form of white crystals.

出典