N-bromobutanimide → HCID 178432447、化合物
反応式
[Br:1]N1C(=O)CCC1=O.[CH3:9][C:10]1[NH:11][CH:12]=[C:13]([CH:15]=[O:16])[N:14]=1>CC#N>[Br:1][C:12]1[N:11]=[C:10]([CH3:9])[NH:14][C:13]=1[CH:15]=[O:16]参加物
4
実験手順
N-bromosuccinimide (0.900 g, 5.0 mmol) was added to a stirred solution of 2-methyl-1H-imidazole-4-carbaldehyde (0.500 g, 5.0 mmol) in CH3CN (50 mL). The reaction mixture was stirred for 3 days in the dark and then concentrated in the presence of silica gel. The absorbed crude material was purified by column chromatography (5-70% EtOAc/hexanes) to afford the title compound (0.334 g, 35%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ ppm 13.34 (br. s., 1H), 9.48 (s, 1H), 2.31 (s, 3H). ES-LCMS: m/z 189.2, 191.2 (M+1).
後処理
- concentrationthen concentrated in the presence of silica gel
- customThe absorbed crude material
- customwas purified by column chromatography (5-70% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-809be7e2e1ff42788a8f94e4aef164b5
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08304419B2
反応ノート
読み込み中…