反応式
Br[CH2:2]/[CH:3]=[CH:4]/[C:5]([OH:7])=O.[CH3:8][N:9]([CH3:18])[C:10]([N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1)=[O:11].CCN(C(C)C)C(C)C.[Cl:28][C:29]1[CH:30]=[C:31]([NH:36][C:37]2[C:38]3[C:45]4[CH2:46][CH2:47][NH:48][CH2:49][C:44]=4[S:43][C:39]=3[N:40]=[CH:41][N:42]=2)[CH:32]=[CH:33][C:34]=1[Cl:35].CCN=C=NCCCN(C)C>C(Cl)Cl.O>[Cl:28][C:29]1[CH:30]=[C:31]([NH:36][C:37]2[C:38]3[C:45]4[CH2:46][CH2:47][N:48]([C:5](=[O:7])/[CH:4]=[CH:3]/[CH2:2][N:15]5[CH2:14][CH2:13][N:12]([C:10]([N:9]([CH3:18])[CH3:8])=[O:11])[CH2:17][CH2:16]5)[CH2:49][C:44]=4[S:43][C:39]=3[N:40]=[CH:41][N:42]=2)[CH:32]=[CH:33][C:34]=1[Cl:35]参加物
8
反応物 5
生成物 1
試薬・触媒・溶媒 2
実験手順
(2E)-4-Bromobut-2-enoic acid (106 mg, 0.64 mmol) and piperazine-1-carboxylic acid dimethylamide (107 mg, 0.68 mmol) were dissolved in DCM (5.0 mL), and DIPEA (111 mg, 0.85 mmol) was added. The mixture was stirred at rt for 2 h. Subsequently, the compound from Example 15A (150 mg, 0.43 mmol), DIPEA (55 mg, 0.43 mmol) and EDCI (82 mg, 0.43 mmol) were added. The reaction mixture was stirred at rt overnight. Then, water was added, and the mixture was extracted three times with DCM. The combined organic layers were dried over sodium sulfate. The solvent was removed in vacuo, and the residue was purified by preparative HPLC to yield 59 mg (24%) of the title compound.
後処理
- stirringThe reaction mixture was stirred at rt overnight
- extractionthe mixture was extracted three times with DCM
- dry with materialThe combined organic layers were dried over sodium sulfate
- customThe solvent was removed in vacuo
- customthe residue was purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-3db0a56a8e02415888246276a89874c5
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524722B2
関連ノート
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