Reaktion #42730

Reaktionsgleichung

Diethyl ether

sodium hydroxide

5-bromo-2-hydroxybenzyl alcohol

acetone

→

title compound

6-Bromo-2,2-dimethyl-4H-benzo[1,3]dioxine

Lösungsmittel

2,2-dimethoxypropane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe organic phase was decanted into a separatory funnel
2. 2
   WaschenThe organic phase was washed with brine
3. 3
   Trocknendried over Na2SO4
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated under reduced pressure

Vorschrift

To 5-bromo-2-hydroxybenzyl alcohol (93 g, 0.46 mol, available from Sigma-Aldrich) in 2.0 L of 2,2-dimethoxypropane was added 700 mL of acetone, followed by zinc chloride (170 g). After stirring for 18 hours, 1.0 M aqueous sodium hydroxide was added until the aqueous phase was basic. Diethyl ether (1.5 L) was added to the slurry and the organic phase was decanted into a separatory funnel. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound as an oil.

Quelle