Methylhydrazine → HCID 86707218、化合物
反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9](=O)[CH:10]=[CH:11][N:12](C)[CH3:13])=[C:4]([F:16])[CH:3]=1.C[NH:18]N>CO>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH:10]=[CH:11][N:12]([CH3:13])[N:18]=2)=[C:4]([F:16])[CH:3]=1参加物
4
実験手順
A mixture of 1-(4-bromo-2,6-difluorophenyl)-3-(dimethylamino)-2-propene-1-one (i.e. the product of Step A, 2.39 g, 8.24 mmol) and methylhydrazine (0.42 g, 9.05 mmol) in methanol (50 mL) was stirred at room temperature overnight. The reaction mixture was then concentrated under reduced pressure, and the residue was purified by medium pressure liquid chromatography on silica gel eluted with 0 to 100% ethyl acetate in hexanes to yield the title compound (0.86 g).
後処理
- concentrationThe reaction mixture was then concentrated under reduced pressure
- customthe residue was purified by medium pressure liquid chromatography on silica gel
- washeluted with 0 to 100% ethyl acetate in hexanes
出典と根拠
- ORDレコード
- ord-97edef35f0e34ee9ba9b3fb1f5f44504
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08815772B2
反応ノート
読み込み中…