反応式
[H-].[Li+].[Al+3].[H-].[H-].[H-].[CH:7]1([NH:10][C:11](=O)[CH2:12][C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[CH2:9][CH2:8]1.O.[OH-].[Na+]>O1CCCC1>[CH:7]1([NH:10][CH2:11][CH2:12][C:13]2[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=2)[CH2:9][CH2:8]1参加物
実験手順
To a suspension of aluminum lithium hydride (0.86 g) in tetrahydrofuran (46 mL) was slowly added dropwise N-cyclopropyl-2-(4-fluorophenyl)acetamide (the compound of Preparation Example 22) (2.17 g) on an iceth. After steirring at room temperature for 8.5 hours, water (0.85 mL), an aqueous solution of 5N sodium hydroxide (0.85 mL) and water (2.5 mL) were poured sequentially, and the solution was stirred at room temperature for 15 hours. The resulting insoluble matter was removed by filtration, the residue that was obtained upon removing the solvent by evaporation was purified by silica gel column chromatography (dichloromethane/methanol), and a crude purifcation product (424 mg) of cyclopropyl-[2-(4-fluorophenyl)ethyl]amine (pale yellow solids) was obtained. From 5-bromothiophene-2-sulfonyl chloride (243 mg) and the above-mentioned amine (354 mg), the title compound (85 mg) was obtained as a colorless oily matter in two steps, which were the same as Preparation Example 41 and Preparation Example 67.
後処理
- customthe compound of Preparation Example 22) (2.17 g) on an iceth
- customThe resulting insoluble matter was removed by filtration
- customthe residue that was obtained
- customupon removing the solvent
- customby evaporation
- customwas purified by silica gel column chromatography (dichloromethane/methanol)
出典と根拠
- ORDレコード
- ord-edeea416ce4041e1bbdbe6970fdbb876
- 出典データセット
- uspto-grants-2007_05
- 特許番号
- US07217723B2
関連ノート
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