p-Toluenesulfonic acid → 5-chloro-3-methyl-3H-imidazo(4,5-b)pyridine
반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH3:9])[C:5]([NH2:10])=[CH:4][CH:3]=1.[CH3:11]C1C=CC(S(O)(=O)=O)=CC=1.CC(=O)OCC>C(OC)(OC)OC>[Cl:1][C:2]1[N:7]=[C:6]2[N:8]([CH3:11])[CH:9]=[N:10][C:5]2=[CH:4][CH:3]=1참가 물질
5
실험 절차
To a solution of 6-chloro-N2-methylpyridine-2,3-diamine (300 mg, 1.9 mmol) in HC(OMe)3 (10 mL) was added TsOH (10 mg) at 22° C. The mixture was stirred for 3 h under reflux until TLC (PE: EA=3:1) showed that the reaction was complete. The mixture was concentrated to get the crude material which was purified by using column chromatography on silica gel to give the desired product (261 mg, 81.6%) as an oil. LCMS (m/z): 168.1 [M+H]+.
후처리
- concentrationThe mixture was concentrated
- customto get the crude material which
- customwas purified
출처 및 근거
- ORD 기록
- ord-cedb94f8bea84501be680c7362e4dc08
- 출처 데이터셋
- uspto-grants-2016_07
- 특허 번호
- US09388173B2
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