反应详情

To a solution of 4.5 g of 2-(2-chloroethoxy)-1-(6-fluorobenzo[b]thiophen-5-yl)ethanone in 45 ml of tetrahydrofuran is added 0.46 g of (R)-5,5-diphenyl-2-methyl-3,4-propano-1,3,2-oxazaborolidine at -10° C., and thereafter, 9.9 ml of 1M borane solution of tetrahydrofuran is dropwise added thereto. The temperature of the resulting mixture is elevated to room temperature, and the mixture is stirred at the same temperature for 1.5 hours, after which 100 ml of water and 100 ml of ethyl acetate are added thereto. The resulting organic layer is separated, washed successively with water and a saturated saline solution and then dried over anhydrous magnesium sulfate. The solvent is then removed from the thus dried layer by distillation under reduced pressure. The residue obtained is purified by a column chromatography [eluent:toluene:ethyl acetate=10:1], to obtain 4.5 g of oily (+)-2-(2-chloroethoxy)-1-(6-fluorobenzo[b]thiophen-5-yl)ethanol.

1. customis elevated to room temperature
2. customThe resulting organic layer is separated
3. washwashed successively with water
4. dry with materiala saturated saline solution and then dried over anhydrous magnesium sulfate
5. customThe solvent is then removed from the thus dried layer by distillation under reduced pressure
6. customThe residue obtained
7. customis purified by a column chromatography [eluent:toluene:ethyl acetate=10:1]