p-Toluenesulfonic acid → 5-chloro-3-methyl-3H-imidazo(4,5-b)pyridine
反応式
[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]=1参加物
5
実験手順
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]+.
後処理
- concentrationThe mixture was concentrated
- customto get the crude material which
- customwas purified
出典と根拠
- ORDレコード
- ord-cedb94f8bea84501be680c7362e4dc08
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388173B2
反応ノート
読み込み中…