반응 #830472
ord-9c0b8e648fec434397aec6ee17ab1fa5
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후처리
- 1기타At the end of this time, the solvent was removed by distillation under reduced pressure
- 2workup.DISSOLUTIONthe resulting solid residue was dissolved in a small amount of methylene chloride
- 3workup.ADDITION20 ml of ethyl acetate was then added to the solution
- 4기타thus obtained
- 5기타to stand at room temperature
- 6기타The crystals which precipitated
- 7여과were collected by filtration
실험 절차
5 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 440 mg of 1-t-butoxycarbonyl-2-{2-[2-(2-phenylethyl)phenoxy]ethyl}piperidine [prepared as described in step (a) above] in 5 ml of dioxane, and the resulting mixture was allowed to stand at room temperature for 2 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting solid residue was dissolved in a small amount of methylene chloride; 20 ml of ethyl acetate was then added to the solution thus obtained, after which it was allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 214 mg (yield 53%) of the title compound as colorless crystals, melting at 95°-97° C.