反応式
[Br-].[C:2]([CH2:4]CC[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)#[N:3].C([N-]C(C)C)(C)C.[Li+].CCCCCCC.[O:41]=[C:42]1[C:50]2[C:45](=[CH:46][CH:47]=[CH:48][CH:49]=2)[C:44](=[O:51])[N:43]1[CH2:52][C:53]1[CH:54]=[C:55]2[C:60](=[CH:61][CH:62]=1)[N:59]=[C:58]([CH2:63][CH2:64][C:65]#N)[CH:57]=[CH:56]2>C1COCC1>[O:51]=[C:44]1[C:45]2[C:50](=[CH:49][CH:48]=[CH:47][CH:46]=2)[C:42](=[O:41])[N:43]1[CH2:52][C:53]1[CH:54]=[C:55]2[C:60](=[CH:61][CH:62]=1)[N:59]=[C:58]([CH:63]=[CH:64][CH2:65][CH2:4][C:2]#[N:3])[CH:57]=[CH:56]2参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
The compound (675.0 mg) obtained in Example 123-1 was suspended in anhydrous THF (30 ml) and cooled with ice. Then, the suspension was added with a 2 mol/l lithium diisopropylamide/heptane solution (0.825 ml), followed by stirring at room temperature for 1 hour. Then, the solution was gradually added with a solution prepared by suspending the compound (327.9 mg) obtained in Example 119-7 in anhydrous THF (20 ml), followed by stirring at room temperature for 3 hours. After completion of the reaction, the solvent was distilled off and the residue was then purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (268.0 mg) as a yellow solid.
後処理
- temperaturecooled with ice
- additionThen, the solution was gradually added with a solution
- customprepared
- stirringby stirring at room temperature for 3 hours
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- customthe residue was then purified through silica gel column chromatography (chloroform/ethyl acetate)
出典と根拠
- ORDレコード
- ord-b44bcb75316b47279e7c895031b81fea
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07833991B2
関連ノート
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