反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:21][CH2:22][C:23]([CH3:25])=[CH2:24])=[C:6]([CH:20]=1)[CH2:7][N:8]([C:11]1[N:16]=[N:15][C:14]([C:17]([OH:19])=O)=[CH:13][CH:12]=1)[CH2:9][CH3:10].Cl.CN(C)CCCN=C=NCC.CN(C1C=CC=CN=1)C.[CH2:47]([S:50]([NH2:53])(=[O:52])=[O:51])[CH2:48][CH3:49]>ClCCl.CN(C1C=CN=CC=1)C.CCO.C(Cl)Cl.O.CC#N>[CH2:47]([S:50]([NH:53][C:17]([C:14]1[N:15]=[N:16][C:11]([N:8]([CH2:7][C:6]2[CH:20]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]=2[O:21][CH2:22][C:23]([CH3:25])=[CH2:24])[CH2:9][CH3:10])=[CH:12][CH:13]=1)=[O:19])(=[O:52])=[O:51])[CH2:48][CH3:49]参加物
9
反応物 4
生成物 1
試薬・触媒・溶媒 4
実験手順
6-[N-(5-Bromo-2-(2-methylprop-2-enyloxy)benzyl)-N-ethylamino]pyridazin-3-carboxylic acid (185 mg, 0.46 mmol) was dissolved in dichloromethane (20 ml), (1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (EDAC), dimethylaminopyridine, (DMAP) (111 mg, 0.91 mmol) and propanesulfonamide (68 mg, 0.55 mmol) were added. The mixture was stirred at ambient temperature under argon overnight, after which TLC (25% water/CH3CN) suggested the reaction was complete. The reaction mixture was loaded directly onto a MPLC column (silica) and the title compound obtained by elution with 5% EtOH/CH2Cl2 then 5% EtOH/0.5% AcOH/CH2Cl2, as a clear oil which solidified on triturating with hexane to give a colourless powder (110 mg, 47%).
出典と根拠
- ORDレコード
- ord-b9cf3959f96f4e03b2eb657f0673b830
- 出典データセット
- uspto-grants-2000_08
- 特許番号
- US06100258
関連ノート
読み込み中…