Water → 2-ethylsulfanylphenyl-N-(5-methyl-2-methylaminopyridin-3-yl)-benzamide
반응식
[CH3:1][C:2]1[CH:3]=[C:4]([NH2:10])[C:5]([NH:8][CH3:9])=[N:6][CH:7]=1.[CH2:11]([S:13][C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16](O)=O)[CH3:12].CCN=C=N[CH2:28][CH2:29][CH2:30]N(C)C.N1C=C[CH:37]=[CH:36][CH:35]=1.[OH2:40]>>[CH2:11]([S:13][C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16]1[CH:28]=[CH:29][CH:30]=[CH:37][C:36]=1[C:35]([NH:10][C:4]1[C:5]([NH:8][CH3:9])=[N:6][CH:7]=[C:2]([CH3:1])[CH:3]=1)=[O:40])[CH3:12]참가 물질
6
반응 조건
- 온도
- 120 °C
실험 절차
A mixture of 5,N2-dimethylpyridin-2,3-diamine (1.13 g), 2-ethylsulfanylbenzoic acid (1.79 g), WSC (1.38 g), and pyridine (20 ml) was stirred with heating under reflux at 120° C. for 2 hours. Into the reaction mixture cooled to room temperature, water was poured, and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to give 1.58 g of 2-ethylsulfanylphenyl-N-(5-methyl-2-methylaminopyridin-3-yl)-benzamide (Compound (1B)-514).
후처리
- temperaturewith heating
- temperatureInto the reaction mixture cooled to room temperature
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-0f387bddc6ba4136ae4cca89b9643380
- 출처 데이터셋
- uspto-grants-2014_10
- 특허 번호
- US08853238B2
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