Reaktion #1258009

Reaktionsgleichung

sodium azide

α-bromoisopropyl 2,2,3,3-tetrafluoro-1,4-benzodioxan-6-yl ketone

dimethyl sulfoxide

→

2,2,3,3-tetrafluoro-1,4-benzodioxan-6-yl ketone

Ausbeute 136.1%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigefollowed by a reaction for two hours at 50° C
2. 2
   Extraktionextracted with diethyl ether
3. 3
   Waschenby washing with water
4. 4
   TrocknenThe organic layer was dried over anhydrous magnesium sulfate
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   SonstigeThe residue was purified by silica gel column chromatography (developing solvent: ethyl acetate/n-hexane=1/19)

Vorschrift

0.65 g of sodium azide was added to a mixture comprising 1.78 g of α-bromoisopropyl 2,2,3,3-tetrafluoro-1,4-benzodioxan-6-yl ketone and 10 ml of dimethyl sulfoxide, followed by a reaction for two hours at 50° C. The reaction mixture was put into water, and extracted with diethyl ether, followed by washing with water. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: ethyl acetate/n-hexane=1/19) to obtain 1.5 g of oily α-azideisopropyl 2,2,3,3-tetrafluoro-1,4-benzodioxan-6-yl ketone. The NMR spectrum data of this product is as follows.

Quelle