Iodine → Methyl 4-amino-3-iodobenzoate
反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.[I:12]I>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][C:11]=1[I:12]参加物
5
実験手順
Methyl 4-aminobenzoate (30.23 g, 200 mmol) was added to a mixture of iodine (60.91 g, 240 mmol) and silver sulfate (81.07 g, 260 mmol) in 1 L of ethanol at room temperature. The mixture was stirred at room temperature for 18 hours, filtered over Celite and the filtrate was evaporated to dryness under reduced pressure. The residue was chromatographed on silica gel (230–400 mesh) and eluted with 1% ethyl acetate in hexane to give 35 g (63%).
後処理
- filtrationfiltered over Celite
- customthe filtrate was evaporated to dryness under reduced pressure
- customThe residue was chromatographed on silica gel (230–400 mesh)
- washeluted with 1% ethyl acetate in hexane
- customto give 35 g (63%)
出典と根拠
- ORDレコード
- ord-f7ee27120d3e45df9a00b6188ab0a4c8
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07098231B2
反応ノート
読み込み中…