Acetone → 1,3-dibutoxybenzene
반응식
[CH2:1](Br)[CH2:2][CH2:3][CH3:4].[C:6](=[O:9])([O-])[O-].[K+].[K+].[C:12]1([CH:19]=[CH:18][CH:17]=[C:15]([OH:16])[CH:14]=1)O.[Cl-].[NH4+].[CH3:22][C:23]([CH3:25])=O>>[CH2:1]([O:16][C:15]1[CH:17]=[CH:18][CH:19]=[C:12]([O:9][CH2:6][CH2:22][CH2:23][CH3:25])[CH:14]=1)[CH2:2][CH2:3][CH3:4]참가 물질
반응 조건
- 온도
- 90 °C
실험 절차
25.5 g of butyl bromide was added to a 150 mL acetone solution of 26.4 g of potassium carbonate and 10.0 g of resorcinol, after which the reaction mixture was stirred for 6 hours at 90° C. 100 mL of a saturated ammonium chloride aqueous solution was poured into the reaction solution under stirring, following by 30 minutes more stirring, after which the solvent was distilled off under reduced pressure. 200 mL of water was added, after which extraction was performed with ethyl acetate (200 mL×3). The organic layer was washed with saturated brine and dried with magnesium sulfate, and the drying agent was then filtered off and the solvent was distilled off under reduced pressure. The residue thus obtained was separated and purified by column chromatography (silica gel 60, mobile phase: hexane/ethyl acetate=95/5 to 1/1; v/v) to obtain 11.0 g of the titled compound (colorless oily substance).
후처리
- stirringunder stirring
- waitfollowing by 30 minutes
- stirringmore stirring
- distillationafter which the solvent was distilled off under reduced pressure
- addition200 mL of water was added
- extractionafter which extraction
- washThe organic layer was washed with saturated brine
- dry with materialdried with magnesium sulfate
- filtrationthe drying agent was then filtered off
- distillationthe solvent was distilled off under reduced pressure
- customThe residue thus obtained
- customwas separated
- custompurified by column chromatography (silica gel 60, mobile phase: hexane/ethyl acetate=95/5 to 1/1; v/v)
출처 및 근거
- ORD 기록
- ord-22af83c0f6c646b08dc6feaa26da6611
- 출처 데이터셋
- uspto-grants-2009_05
- 특허 번호
- US07528124B2
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