반응식
[C:1]([CH:3]([CH:7]1[C:11]([Cl:12])=[C:10](Cl)C(=O)O1)[C:4]([NH2:6])=[O:5])#[N:2].[NH2:15][CH2:16][C:17]1[CH:18]=[C:19]([S:23]([N:26]([CH3:28])[CH3:27])(=[O:25])=[O:24])[CH:20]=[CH:21][CH:22]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[ClH:12].[Cl:12][C:11]1[CH:7]=[C:3]([C:4]([NH2:6])=[O:5])[C:1](=[NH:2])[N:15]([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([S:23](=[O:25])(=[O:24])[N:26]([CH3:27])[CH3:28])[CH:18]=2)[CH:10]=1참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 70 °C
실험 절차
(Step 2) To a suspension of 2-cyano-2-(3,4-dichloro-5-oxo-2,5-dihydrofuran-2-yl)acetamide (0.73 g) and 3-(aminomethyl)-N,N-dimethylbenzenesulfonamide obtained in Step 1 (1.0 g) in ethanol (10 ml) was added potassium carbonate (0.65 g) at room temperature, and the mixture was stirred overnight at 70° C. The reaction solution was filtered through celite. The solvent was evaporated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate:hexane=7:3→1:0). 4N Hydrochloride-ethyl acetate solution (1 ml) was added to the obtained yellow oil, and the precipitated crystals were collected by filtration, and recrystallized to give the title compound (306 mg).
후처리
- filtrationThe reaction solution was filtered through celite
- customThe solvent was evaporated under reduced pressure
- customThe residue was purified by basic silica gel column chromatography (ethyl acetate:hexane=7:3→1:0)
- addition4N Hydrochloride-ethyl acetate solution (1 ml) was added to the obtained yellow oil
- filtrationthe precipitated crystals were collected by filtration
- customrecrystallized
출처 및 근거
- ORD 기록
- ord-98c41bf1a73c4337898bd81d5f263ce2
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08481569B2
연결된 노트
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