N-bromobutanimide → N-{5-[8-(1-Ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazin-3-yl]-4-methyl-oxazol-2-yl}-dimethylamine
반응식
[CH2:1]([CH:3]([C:6]1[C:7]2[N:8]([C:13]([C:17]3[O:21][CH:20]=[N:19][C:18]=3[CH3:22])=[C:14]([CH3:16])[N:15]=2)[N:9]=[C:10]([CH3:12])[CH:11]=1)[CH2:4][CH3:5])[CH3:2].C1[C:28](=O)[N:27](Br)[C:25](=O)C1>C(Cl)Cl>[CH2:1]([CH:3]([C:6]1[C:7]2[N:8]([C:13]([C:17]3[O:21][C:20]([N:27]([CH3:28])[CH3:25])=[N:19][C:18]=3[CH3:22])=[C:14]([CH3:16])[N:15]=2)[N:9]=[C:10]([CH3:12])[CH:11]=1)[CH2:4][CH3:5])[CH3:2]참가 물질
4
실험 절차
230 mg of 8-(1-Ethyl-propyl)-2,6-dimethyl-3-(4-methyl-oxazol-5-yl)-imidazo[1,2-b]pyridazine (0.77 mmol) is dissolved in 20 ml of CH2Cl2 and 178 mg of NBS (1.0 mmol) is added. The reaction mixture is stirred at room temperature overnight. The reaction mixture is washed with sat. Na2S2O3, sat. NaCl, dried over Na2SO4 and evaporated. The crude product is applied onto a silica-gel chromatography column (Hexane:AcOEt=3:1) to give 36 mg of the title compound. Yield 12%. mass spectrum (m/e): 378 (M+1). 1H-NMR (CDCl3): 6.82 (s, 1H), 3.39 (m, 1H), 2.58 (s, 3H), 2.53 (s, 3H), 2.26 (s, 3H), 1.85 (m, 1H), 0.89 (t, J=7.4 Hz, 6H).
후처리
- washThe reaction mixture is washed with sat. Na2S2O3, sat. NaCl
- dry with materialdried over Na2SO4
- customevaporated
출처 및 근거
- ORD 기록
- ord-70bb00d547da40ecaf62391e8f974291
- 출처 데이터셋
- uspto-grants-2009_11
- 특허 번호
- US07612067B2
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