Reaktion #676370

Reaktionsgleichung

Ammonium chloride

ethylmagnesium bromide

5-bromopicolinonitrile

boron trifluoride diethyl etherate

→

1-(5-bromopyridin-2-yl)cyclopropanamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe solution was extracted with ethyl acetate for three times
2. 2
   SonstigeThe organic layers were collected
3. 3
   Waschenwashed with brine
4. 4
   Trocknendried over sodium sulfate
5. 5
   EinengenAfter concentration the crude product
6. 6
   Sonstigewas purified by SiO2 column

Vorschrift

To a mixture of 5-bromopicolinonitrile (1.82 g, 10.0 mmol), tetrapropoxytitanium (3.26 ml, 11.0 mmol) and boron trifluoride diethyl etherate (2.51 ml 20.0 mmol) at 0° C. was added ethylmagnesium bromide (1.0M in ether, 22 ml, 22.0 mmol) The resulting solution was allowed to stir at it for 3 h. Ammonium chloride solution was added and the solution was extracted with ethyl acetate for three times. The organic layers were collected and washed with brine and dried over sodium sulfate. After concentration the crude product was purified by SiO2 column.

Quelle