Methylhydrazine → HCID 136200892, 화합물
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-1894b90a44964114a499aa094415f0bf
- 출처 데이터셋
- uspto-grants-2014_07
- 특허 번호
- US08772293B2
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