Sulfuric Acid → 1-(3-tert-Butoxyphenyl)ethan-1-one
反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1.[CH3:11][C:12](=[CH2:14])[CH3:13].OS(O)(=O)=O>ClCCl>[C:12]([O:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1)([CH3:14])([CH3:13])[CH3:11]参加物
5
実験手順
A mixture of 3'-hydroxyacetophenone (22.64 g), isobutylene (300 mL) and concentrated H2SO4 (1 mL) in dry dichloromethane (310 mL) was stirred in a sealed pressure vessel at room temperature for 3 days. After the reaction vessel was vented, the organic phase was washed (10% NaOH, water and brine), dried and evaporated to an oil (25.95 g) which was purified by chromatography, eluting with dichloromethane:ethyl acetate, to give 3'-tert-butoxyacetophenone (22.62 g); TLC: Rf =0.55, ethyl acetate:dichloromethane (3:97); MS: m/z=193(M+1).
後処理
- washthe organic phase was washed (10% NaOH, water and brine)
- customdried
- customevaporated to an oil (25.95 g) which
- customwas purified by chromatography
- washeluting with dichloromethane
出典と根拠
- ORDレコード
- ord-b2fda2dafd5646c785dadc253ef0ea92
- 出典データセット
- uspto-grants-1996_05
- 特許番号
- US05521179
反応ノート
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