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].CN(C1C=CC=CN=1)C.[CH3:35][C:36]1[C:40]([S:41]([NH2:44])(=[O:43])=[O:42])=[C:39]([CH3:45])[O:38][N:37]=1.O.CO>ClCCl.C(O)C.ClCCl>[CH3:35][C:36]1[C:40]([S:41]([NH:44][C:17]([C:14]2[N:15]=[N:16][C:11]([N:8]([CH2:7][C:6]3[CH:20]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]=3[O:21][CH2:22][C:23]([CH3:25])=[CH2:24])[CH2:9][CH3:10])=[CH:12][CH:13]=2)=[O:19])(=[O:43])=[O:42])=[C:39]([CH3:45])[O:38][N:37]=1참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
6-[N-(5-Bromo-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]pyridazine-3-carboxylic acid (example 2, compound 15) (187 mg, 0.46 mmol) was dissolved in dichloromethane (20 ml) and (1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (EDAC),(133 mg, 0.69 mmol), dimethylaminopyridine (DMAP) (113 mg, 0.92 mmol) and 3,5-dimethylisoxazol-4-ylsulfonamide (98 mg, 0.56 mmol) were added. The mixture was stirred at ambient temperature under argon for 72 hours, after which TLC (25% water/methanol) suggested the reaction was complete. The reaction mixture was loaded directly onto a MPLC column (silica) and the title compound obtained by elution 2.5% ethanol/dichloromethane followed by 0.5% acetic acid/2.5% ethanol/dichloromethane as a gum which was triturated with hexane to give the title product as a solid (98 mg, 38%).
출처 및 근거
- ORD 기록
- ord-183d20e51122487686eb6e60b8af2cf2
- 출처 데이터셋
- uspto-grants-2000_08
- 특허 번호
- US06100258
연결된 노트
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