Sulfuryl chloride → 1H-Pyrrolo[2,3-b]pyridine-3-acetonitrile, 2-chloro-
反応式
[C:1]([CH2:3][C:4]1[C:12]2[C:7](=[N:8][CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1)#[N:2].S(Cl)([Cl:16])(=O)=O>C(O)(=O)C>[Cl:16][C:5]1[NH:6][C:7]2=[N:8][CH:9]=[CH:10][CH:11]=[C:12]2[C:4]=1[CH2:3][C:1]#[N:2]参加物
4
実験手順
3-cyanomethylpyrrolo[2,3-b]pyridine (1,55 g, 0.098 mol) was treated in 5 ml acetic acid with an equimolecular amount of sulfurylchloride at 0° C. for 5 min. The mixture was allowed to warm to room temperature and was stirred 5 min. After evaporation the residue was dissolved in methylen chloride and was treated with bicarbonate. The organic layer was separated, dried over Na2SO4 and the solvent was removed under reduced pressure. Chromatography on silica gel eluting with ethyl acetate gave the desired product. (0,4 g 21%).
後処理
- customAfter evaporation the residue
- dissolutionwas dissolved in methylen chloride
- additionwas treated with bicarbonate
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- customthe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-35ec616ca9f1410dbe3bae3a04a93e87
- 出典データセット
- uspto-grants-1995_08
- 特許番号
- US05439917
反応ノート
読み込み中…