Ammonium fluoride → Methyl 5-hydroxy-2-methoxybenzoate
反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([O:13][Si](C(C)(C)C)(C)C)=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6].[F-].[NH4+]>CO>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6]参加物
4
実験手順
Combine methyl 2-methoxy-5-(t-butyldimethylsilyloxy)benzoate (11.1 g. 37.4 mmol) and ammonium fluoride (6.94 g, 0.187 mmol) in methanol (150 mL). Heat to reflux. After 1 hour, evaporate in vacuo to give a residue. Partition the residue between ethyl acetate and water, separate the layers, extract the organic layer with water and then brine. Dry the organic layer over MgSO4, filter, and evaporate in uacuo to give methyl 2-methoxy-5-hydroxybenzoate: mp; 110-112° C. Rf=0.27 (silica gel, 5% ethyl acetate/hexane).
後処理
- temperatureHeat to reflux
- customevaporate in vacuo
- customto give a residue
- customPartition the residue between ethyl acetate and water
- customseparate the layers
- extractionextract the organic layer with water
- dry with materialDry the organic layer over MgSO4
- filtrationfilter
- customevaporate in uacuo
出典と根拠
- ORDレコード
- ord-cc63f7f2d2c947808406a91e56a6584e
- 出典データセット
- uspto-grants-2001_02
- 特許番号
- US06194406B1
反応ノート
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