反応式
[CH2:1]([CH:3]([CH2:9][CH3:10])/[CH:4]=[CH:5]/[C:6]([OH:8])=O)[CH3:2].C(N(C(C)C)CC)(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:44][C:45]1[CH:54]=[C:53]([N:55]2[CH2:60][CH2:59][NH:58][CH2:57][CH2:56]2)[C:52]2[C:47](=[CH:48][C:49]([C:61]([F:64])([F:63])[F:62])=[CH:50][CH:51]=2)[N:46]=1>CN(C=O)C>[CH2:9]([CH:3]([CH2:1][CH3:2])/[CH:4]=[CH:5]/[C:6]([N:58]1[CH2:59][CH2:60][N:55]([C:53]2[C:52]3[C:47](=[CH:48][C:49]([C:61]([F:64])([F:62])[F:63])=[CH:50][CH:51]=3)[N:46]=[C:45]([CH3:44])[CH:54]=2)[CH2:56][CH2:57]1)=[O:8])[CH3:10]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
(E)-4-Ethyl-hex-2-enoic acid (21.3 mg, 0.15 mmol) was dissolved in DMF (350 μl), diisopropylethylamine was added (26 μl, 0.15 mmol) followed by HATU (57 mg, 0.15 mmol dissolved in 0.25 ml DMF). The mixture was stirred at room temperature for 15 minutes, then 2-methyl-4-piperazin-1-yl-7-(trifluoromethyl)quinoline (44 mg, 0.15 mmol, dissolved in 1 ml DMF) was added and stirring was continued overnight. The mixture was evaporated under reduced pressure, the residue was dissolved in dichloromethane, the solution was washed with 5% sodium bicarbonate solution and water, evaporated to dryness under reduced pressure. The residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 20.3 mg (0.48 mmol, 32.3%) of a solid.
後処理
- stirringstirring
- waitwas continued overnight
- customThe mixture was evaporated under reduced pressure
- dissolutionthe residue was dissolved in dichloromethane
- washthe solution was washed with 5% sodium bicarbonate solution and water
- customevaporated to dryness under reduced pressure
- customThe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)
出典と根拠
- ORDレコード
- ord-23d9052b54ca46bc91e6c5c92c1738e0
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08883791B2
関連ノート
読み込み中…