144809-26-7 synthesis

Yield:144809-26-7 99%

Reaction Conditions:

with triethylamine in dichloromethane at 5 - 20; for 1.5 h;

Steps:

1b EXAMPLE lb; Production [OF 2- (5-ETHYL-2-PYRIDYL) ETHYL METLLANESULFONATE]

A 500 ml two-necked flask equipped with a magnetic stirring bar and thermometer was charged with 10 g (0.0661 mol) of 2- (5-ethyl-2-pyridyl) ethanol, [130] ml of methylene chloride, and 9.82 g [(0.] 09 mol) of triethylamine at room temperature. The mixture was cooled to [5 °C] and to the cooled mixture was added slowly 12.43 g (0.086 mol) of [METHANESULFONYL] chloride at [5'C OVER] 30 minutes. The reaction mixture was stirred at temperatures ranging from 15 to [20 °C] for 1 hour. The precipitate was filtered off and the filtrate was washed first with 100 ml of water, then 100 ml of 5 wt % of sodium hydrogen carbonate, and 100 ml of water. The organic layer was dried over 10 g of anhydrous sodium sulfate. Sodium sulfate was filtered off and the filtrate was concentrated under reduced pressure to give 15 g of the product, [2- (5-ETHYL-2-PYRIDYL)] ethyl [METHANESULFONATE,] as an oil (yield [99%).]

References:

WO2004/810,2003,A1 Location in patent:Page 6-7