반응 #67962
ord-1a20acba42b44c2fb88c7da546c2a2e8
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후처리
- 1기타the solvent was removed under reduced pressure
- 2기타The residue thus obtained
- 3기타The aqueous layer was separated
- 4workup.ADDITIONethyl acetate was added
- 5기타The organic layer was separated
- 6건조dried over potassium carbonate
- 7기타the solvent was removed under reduced pressure
실험 절차
To 0.60 g of 1-tert-butyl 3-ethyl 4-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-1,3-dicarboxylate, 12 mL of 10 mol/L hydrogen chloride/ethanol was added, and the mixture was stirred for 2 hours, and then the solvent was removed under reduced pressure. The residue thus obtained was added with water and ethyl acetate. The aqueous layer was separated, ethyl acetate was added thereto, and the resultant solution was adjusted to pH 14 with a 5 mol/L aqueous sodium hydroxide solution. The organic layer was separated and dried over potassium carbonate, and the solvent was removed under reduced pressure to obtain 0.34 g of a brown oily substance, ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-2-carboxylate.