反応式
[I-].[Na+].Cl[Si](C)(C)C.O[CH:9]([C:21]1[O:22][C:23]([C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([C:32]([F:35])([F:34])[F:33])[CH:27]=2)=[CH:24][CH:25]=1)[C:10]1[CH:20]=[CH:19][C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][CH:11]=1.O>C(#N)C>[F:34][C:32]([F:33])([F:35])[C:28]1[CH:27]=[C:26]([C:23]2[O:22][C:21]([CH2:9][C:10]3[CH:20]=[CH:19][C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][CH:11]=3)=[CH:25][CH:24]=2)[CH:31]=[CH:30][CH:29]=1参加物
6
実験手順
Sodium iodide (0.49 g) was suspended in acetonitrile (2 mL), and the suspension was cooled in an ice bath. Chlorotrimethylsilane (0.42 mL), and then a solution of the compound (0.26 g) obtained in Example 222b in acetonitrile (2 mL) were added. The reaction mixture was stirred at the same temperature for 30 min, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (0.22 g) as an oil.
後処理
- temperaturethe suspension was cooled in an ice bath
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)
出典と根拠
- ORDレコード
- ord-9b2caf62981d42d98926b957a431c752
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08461348B2
関連ノート
読み込み中…