反応式
[CH2:1]([NH:3][C:4](=[O:12])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:11])[CH3:2].CN(CCN(C)C)C.[Li]C(CC)C.[Mg+2].[Br-].[Br-].CCOCC.C(OO[O:44][C:45]([CH3:48])([CH3:47])[CH3:46])(=O)C1C=CC=CC=1>C1COCC1>[CH2:1]([NH:3][C:4](=[O:12])[C:5]1[C:10]([O:44][C:45]([CH3:48])([CH3:47])[CH3:46])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:11])[CH3:2]参加物
8
反応物 6
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of the compound of Example f (3.7 g, 20 mmol) and TMEDA (6.0 mL, 40 mmol) in anhydrous THF (100 mL) at -78° C. under nitrogen was added dropwise 1.3M s-BuLi (34 mL, 44 mmol). After 30 min MgBr2.Et2O (15.5 g, 60 mmol) was added, and the solution was warmed to ambient temperature, then cooled to -78° C. and stirred for 1 h. t-Butylperoxy benzoate (4.3 g, 22 mmol) was added, and the solution was warmed to -30° C. and worked up in the usual manner. Purification by HPLC with 3:17 ethyl acetate/hexanes gave 1.7 g of the desired compound as a white solid, a yield of 33%. m.p. 126-127° C.
後処理
- temperaturecooled to -78° C.
- additionwas added
- temperaturethe solution was warmed to -30° C.
- customPurification by HPLC with 3:17 ethyl acetate/hexanes
出典と根拠
- ORDレコード
- ord-c11d28e8f9484ad18488f0e7a435cc73
- 出典データセット
- uspto-grants-2000_02
- 特許番号
- US06028101
関連ノート
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