Methanol, 1,1-diethoxy-, 1-acetate → 5-Bromo-(1,2,4)triazolo(4,3-a)pyridine
反応式
[Br:1][C:2]1[N:7]=[C:6]([NH:8][NH2:9])[CH:5]=[CH:4][CH:3]=1.[C:10](OC(OCC)OCC)(=O)C>CCCCC>[Br:1][C:2]1[N:7]2[CH:10]=[N:9][N:8]=[C:6]2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
A solution of (6-bromopyridin-2-yl)hydrazine (500 mg, 2.66 mmol) in diethoxymethyl acetate (2.5 mL) was stirred at room temperature for 18 hours. The reaction mixture was diluted with pentane and filtered. The precipitate was washed with pentane and dried at 50° C. under vacuum for 1 hour to give 5-bromo-[1,2,4]triazolo[4,3-a]pyridine as a beige solid (410 mg, 78%). 1H NMR (400 MHz, CHCl3-d): δ 8.98 (s, 1 H); 7.83 (dt, J=9.2, 0.9 Hz, 1 H); 7.22 (dd, J=9.2, 7.0 Hz, 1 H); 7.09 (dd, J=7.0, 0.9 Hz, 1 H).
後処理
- filtrationfiltered
- washThe precipitate was washed with pentane
- customdried at 50° C. under vacuum for 1 hour
出典と根拠
- ORDレコード
- ord-f045edc9168a4d579f5e77feb4960888
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08394796B2
反応ノート
読み込み中…