5 h concentration under reduced pressure and transfer of the resulting oil to a cooled stirring solution of naoh 3 0 n 1 1 eq 28 l in a 100 l extractor was followed by addition of 30 l of mtbe and the phases were separated the organic layer was washed with 30 l of 2 n hcl and again with 10 l of 2 nhcl the aqueous layers were then cooled 9 u00b0 c and 10 n naoh was added until the ph was 13 t u00b0 21 u00b0 c to this solution was added 25 l of mtbe and the layers were cut finally the aqueous layer was back extracted with 10 l of mtbe quantitative hplc assay revealed 98 yield and gt 99 7 purity of a 9 used as is a subsequent reaction data for a 9 lrms m h 225 1 a 3 l three necked round bottomed flask equipped with a septum nitrogen inlet adapter mechanical stirrer and thermocouple was charged with a 5 87 0 g 2 5 difluoropyridine 30 0 g and 870 ml of dmso 110 ppm water at room temperature 23 u00b0 c sodium t butoxide 50 1 g was added portion wise over 4 min keeping the internal temperature below 29 u00b0 c the resulting reaction mixture was stirred at room temperature ea 25 u00b0 c until hplc analysis indicated less than 5 difluoropyridine compared to the desired product agilent eclipse xdb c18 4 6 u00d7 150 mm column 35 u00b0 c mobile phase a 0 1 h 3 po 4 water b acetonitrile linear gradient time 0 95 a 5 b time 6 min 5 a 95 b time 10 min 5 a 95 b flow rate 1 5 ml min uv 210 tun a 5 rt.