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[C:1]([C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)([CH2:4][C:5]([CH3:8])([CH3:7])[CH3:6])([CH3:3])[CH3:2].[C:16](O)([CH3:19])([CH3:18])[CH3:17]>C(O)(C(F)(F)F)=O.O>[C:16]([C:13]1[CH:14]=[C:9]([C:1]([CH2:4][C:5]([CH3:8])([CH3:7])[CH3:6])([CH3:2])[CH3:3])[CH:10]=[CH:11][C:12]=1[OH:15])([CH3:19])([CH3:18])[CH3:17]참가 물질
실험 절차
4-t-octylphenol (160 g, 0.78 mole) was dissolved in 400 ml anhydrous TFA. T-butyl alcohol (94.3 g, 1.27 mole) was added with stirring. The mixture was stoppered and stirred for 24 hours at ambient (~22° C.) temperature. This solution was diluted with 600 ml water, and the resulting upper organic layer was isolated in a separatory funnel. The crude product, 2-t-butyl-4-t-octylphenol, was dried over anhydrous magnesium sulfate and purified by eluting 35 g of the mixture with 70:30 hexanes:dichloromethane (v/v) in a 5×20 cm silica column, then eluted with 300 to 700 ml of solvent and collected in aliquots of 50 ml. Aliquots showing a single spot by TLC on silica eluted with 70:30 hexanes:dichloromethane (v/v) were combined and rotoevaporated to a thick syrup for a yield of 54%.
후처리
- stirringstirred for 24 hours at ambient (~22° C.) temperature
- customthe resulting upper organic layer was isolated in a separatory funnel
- dry with materialThe crude product, 2-t-butyl-4-t-octylphenol, was dried over anhydrous magnesium sulfate
- custompurified
- washby eluting 35 g of the mixture with 70:30 hexanes
- washdichloromethane (v/v) in a 5×20 cm silica column, then eluted with 300 to 700 ml of solvent
- customcollected in aliquots of 50 ml
- washeluted with 70:30 hexanes
출처 및 근거
- ORD 기록
- ord-843e434730ac4e9cbf0db26c285ece4a
- 출처 데이터셋
- uspto-grants-1993_11
- 특허 번호
- US05266283
연결된 노트
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