Chlorosuccinimide → HCID 178499148、化合物
反応式
[Cl:1]N1C(=O)CCC1=O.[NH:9]1[CH:13]=[C:12]([C:14]([O:16][CH3:17])=[O:15])[N:11]=[CH:10]1>CC#N>[Cl:1][C:13]1[N:9]=[CH:10][NH:11][C:12]=1[C:14]([O:16][CH3:17])=[O:15]参加物
4
実験手順
N-chlorosuccinimide (0.318 g, 2.4 mmol) was added to a stirred solution of methyl 1H-imidazole-4-carboxylate (0.300 g, 2.4 mmol) in CH3CN (16 mL). The reaction mixture was stirred for 12 h in the dark and then concentrated. The white residue was taken up in EtOAc, satd. aqueous Na2S (10 mL) was added and the solution was stirred for 15 min. The organic layer was isolated, dried (Na2SO4), concentrated and the crude product was purified by column chromatography (20-70% EtOAc/hexanes) to afford the title compound (0.061 g, 16%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 11.05 (br. s., 1H), 7.85 (s, 1H), 3.81 (s, 3H). ES-LCMS: m/z 160.9, 162.9 (M+1).
後処理
- concentrationthen concentrated
- additionaqueous Na2S (10 mL) was added
- stirringthe solution was stirred for 15 min
- customThe organic layer was isolated
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customthe crude product was purified by column chromatography (20-70% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-c888d540238342c6ae229826e62701f6
- 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…