Reaktion #1519140

Reaktionsgleichung

Oxone

sodium hydrogen carbonate

2,3-dihydro-1-benzoxepin

→

expected product

1a,2,3,8b-Tetrahydrooxireno[d][1]benzoxepin

Lösungsmittel

water

—

mixture

ethyl acetate water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the end of the addition
2. 2
   workup.WAITis carried out for a further hour
3. 3
   Sonstigethe organic phase is separated off
4. 4
   ExtraktionThe aqueous phase is again extracted with 10 ml of ethyl acetate
5. 5
   Waschenthe combined organic phases are washed with water
6. 6
   Sonstigedried
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated to dryness

Vorschrift

To 0.5 g of 2,3-dihydro-1-benzoxepin (3.42 mmol), prepared according to the method described in J. Org. Chem., 1969, 34 (1), 207, dissolved in 30 ml of a mixture of ethyl acetate/water 50/50, there are added 1.44 g of sodium hydrogen carbonate (17.1 mmol) and then, over 1 hour, a solution of 2.1 g of Oxone® (3.42 mmol) in 15 ml of water. After the end of the addition, stirring is carried out for a further hour and then the organic phase is separated off. The aqueous phase is again extracted with 10 ml of ethyl acetate, and the combined organic phases are washed with water, dried, filtered and evaporated to dryness to yield the expected product in the form of an oil.

Quelle