Methylhydrazine → HCID 136200892、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH:7]=[CH:6][C:5]2=O.[CH3:13][NH:14][NH2:15].B(F)(F)F.CCOCC>C(O)C>[Br:1][C:2]1[CH:11]=[CH:10][C:9]([OH:8])=[C:4]([C:5]2[N:14]([CH3:13])[N:15]=[CH:7][CH:6]=2)[CH:3]=1参加物
5
実験手順
To a suspension of 6-bromochromone (1.58 g, 0.0070 mol) in ethanol (30 mL) was added methylhydrazine (0.41 mL, 0.0077 mol) and boron trifluoride etherate (1.15 mL, 0.0091 mol). The reaction was heated to reflux for 22 hours. After cooling, the reaction was concentrated in vacuo and the residue purified by automated flash column chromatography using a 0-100% ethyl acetate/hexanes gradient. This provided the title compound (0.79 g, 44%) as a light yellow solid.
後処理
- temperatureThe reaction was heated
- temperatureto reflux for 22 hours
- temperatureAfter cooling
- concentrationthe reaction was concentrated in vacuo
- customthe residue purified by automated flash column chromatography
出典と根拠
- ORDレコード
- ord-1894b90a44964114a499aa094415f0bf
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772293B2
反応ノート
読み込み中…