Ammonia → 2-(Diphenylphosphanyl)-6-methoxypyridine

Participants

Reaction Conditions

Reaction Steps

2.7 g Sodium was added to 100 ml liquid ammonia at -80 ° C., and then 15.2 g triphenylphosphine was added in 6 portions with stirring. The solution was slowly warmed to -40° C., kept at that temperature for 30 min, and then cooled again to -80° C. Then, 3.1 g ammonium chloride was added to the stirred solution, followed by 10.9 g 2-bromo-6-methoxypyridine in three portions. The cooling bath was removed and the ammonia was allowed to evaporate. The residue was worked up with water/dichloromethane as described in preparation 1. Crystallization from hexane afforded 7 g of a somewhat impure product (characterized by 31P NMR: dq =-4.4 ppm) which was used as such in the following Examples.

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