N-Iodosuccinimide → HCID 178470396、化合物
反応式
[CH2:1]([O:3][C:4]([C:6]1[NH:7][CH:8]=[N:9][C:10]=1[CH3:11])=[O:5])[CH3:2].C1C(=O)N([I:19])C(=O)C1>C1COCC1>[CH2:1]([O:3][C:4]([C:6]1[NH:7][C:8]([I:19])=[N:9][C:10]=1[CH3:11])=[O:5])[CH3:2]参加物
4
実験手順
A solution of 5 g 5-Methyl-3H-imidazole-4-carboxylic acid ethyl ester and 7.2 g NIS in 50 ml THF were refluxed for 10 h. After cooling, the solvent was removed under reduced pressure and the residue taken-up in ethyl acetate, washed with sat. NaS2O3 solution and dried over MgSO4. After removal of the solvent under reduced pressure the product was purified by recrystallisation from ethyl acetate. Yield: 7 g
後処理
- temperatureAfter cooling
- customthe solvent was removed under reduced pressure
- washthe residue taken-up in ethyl acetate, washed with sat. NaS2O3 solution
- dry with materialdried over MgSO4
- customAfter removal of the solvent under reduced pressure the product
- customwas purified by recrystallisation from ethyl acetate
出典と根拠
- ORDレコード
- ord-cc9326ec9b034b019e7134ef7508ca68
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07358268B2
反応ノート
読み込み中…