反应详情

In 11 ml of N,N-dimethylformamide was dissolved 2.29 g of 3-[p-(3-chloro-1-hydroxy-2-methylpropyl)benzyl]pyridine, and to the resulting solution was added 1.36 g of sodium acetate, after which the resulting mixture was subjected to reaction under reflux for 2 hours. The solvent was removed by distillation under reduced pressure, and to the residue thus obtained were added 20 ml of a saturated aqueous sodium chloride solution and 20 ml of ethyl acetate. The organic layer was separated, washed with 10 ml of water, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and the residue thus obtained was purified by a column chromatography [Wako Silica Gel C-200, eluant: chloroform] to obtain 910 mg (yield 36.7%) of colorless, oily 3-[p-(3-acetoxy-1-hydroxy-2-methylpropyl)benzyl]pyridine.

1. customafter which the resulting mixture was subjected to reaction
2. temperatureunder reflux for 2 hours
3. customThe solvent was removed by distillation under reduced pressure
4. customto the residue thus obtained
5. customThe organic layer was separated
6. washwashed with 10 ml of water
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was removed by distillation under reduced pressure
9. customthe residue thus obtained
10. customwas purified by a column chromatography [Wako Silica Gel C-200, eluant: chloroform]