反応式
[Si]([O:8][CH2:9][C:10]1[C:15]([F:16])=[CH:14][C:13]([B:17]([OH:19])[OH:18])=[CH:12][C:11]=1[F:20])(C(C)(C)C)(C)C>C(O)(=O)C>[F:16][C:15]1[CH:14]=[C:13]([B:17]([OH:18])[OH:19])[CH:12]=[C:11]([F:20])[C:10]=1[CH2:9][OH:8]参加物
3
反応条件
- 温度
- 40 °C
実験手順
[4-({[tert-Butyl(dimethyl)silyl]oxy}methyl)-3,5-difluorophenyl]boronic acid (19.3 g, 63.9 mmol; crude material, prepared by the method of Hattori, Bioorg. Med. Chem. 2006, 14, 3258-3262) was dissolved in 400 mL aqueous acetic acid (66%) and stirred at 40° C. for 5 h. The solution was then evaporated under reduced pressure, and the residue was purified by flash chromatography over silica gel (gradient elution from 0% to 2% methanol in dichloromethane) to give 3.46 g (25% of th., LC-MS purity 87%) of the title compound.
後処理
- customcrude material, prepared by the method of Hattori, Bioorg
- customThe solution was then evaporated under reduced pressure
- customthe residue was purified by flash chromatography over silica gel (gradient elution from 0% to 2% methanol in dichloromethane)
出典と根拠
- ORDレコード
- ord-bdb04ad6ea5f41c997219a58bf2c93f2
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040691B2
関連ノート
読み込み中…