Ethyl Acetate → HCID 86062444, compound

Participants

Reaction Steps

1.33 g of 60% sodium hydride was introduced to 15 ml of tetrahydrofuran, the mixture was cooled down to 5 degree centigrade, and then 5.84 g of 1,1,1,3,3,3-hexafluoro-2-propanol wad added dropwise thereto. The resulting solution was stirred at 5 degree centigrade for 30 minutes, and then 3.0 g of 2-chloro-4-methyl-5-nitropyridine dissolved in 10 ml of tetrahydrofuran was added dropwise thereto, and stirred at room temperature for 3 hours. The solution was allowed to stand at room temperature for 3 days, and then ethyl acetate and water were added thereto. An organic layer was separated, washed with saturated salt water, and dried over anhydrous magnesium sulfate. Then, the solvent was removed under a reduced pressure to obtain a residue. The resulting residue was purified by silica gel column chromatography using an eluent (development solvent; hexane ethyl acetate=10:1) to obtain 4.5 g of the desired product (Yield: 80%) as yellow oil.

Provenance & Evidence