반응식
[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]참가 물질
9
반응물 4
생성물 1
시약·촉매·용매 4
실험 절차
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%).
출처 및 근거
- ORD 기록
- ord-b9cf3959f96f4e03b2eb657f0673b830
- 출처 데이터셋
- uspto-grants-2000_08
- 특허 번호
- US06100258
연결된 노트
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