Reaktion #482017

Reaktionsgleichung

3,6-dichloro-2-methylbenzyl bromide

N-methylmorpholine N-oxide

→

3,6-dichloro-2-methylbenzaldehyde

Lösungsmittel

acetonitrile

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe precipitate is filtered off with suction
2. 2
   workup.ADDITION250 g (0.42 mol) of 20% strength NMO in acetonitrile are then added at 40° C
3. 3
   workup.STIRRINGThe reaction mixture is stirred at 40° C. for 1 h
4. 4
   Einengenconcentrated under reduced pressure
5. 5
   Waschenthe mixture is washed three times with 250 ml of water
6. 6
   Trocknendried over Na2SO4
7. 7
   Einengenconcentrated under reduced pressure

Vorschrift

67.4 g (0.19 mol) of 72.2% pure 3,6-dichloro-2-methylbenzyl bromide is initially charged in 280 ml of acetonitrile. At 0-5° C., a solution of 54.0 g (0.46 mol) of N-methylmorpholine N-oxide and 280 ml of acetonitrile is added over a period of 25 min, and the mixture is stirred at 0-8° C. for 1 h. The precipitate is filtered off with suction and taken up in 280 ml of acetonitrile, and 250 g (0.42 mol) of 20% strength NMO in acetonitrile are then added at 40° C. The reaction mixture is stirred at 40° C. for 1 h and concentrated under reduced pressure, the residue is taken up in 250 ml of methylene chloride and the mixture is washed three times with 250 ml of water, dried over Na2SO4 and concentrated under reduced pressure. This gives 32.9 g of a product which is 92.6% pure.

Quelle