Iodine → Methyl 2-amino-4-chloro-5-iodobenzoate
反応式
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:5]=1[NH:11]C(=O)C.[I:16]I>FC(F)(F)S([O-])(=O)=O.[Ag+]>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([I:16])[C:7]([Cl:10])=[CH:6][C:5]=1[NH2:11]参加物
4
実験手順
To a suspension of 2-acetylamino-4-chlorobenzoic acid methyl ester (2.0 g in 80 mL of dry chloroform) and 2.5 g silver trifluoromethanesulfonate was added iodine (2.87 g in 40 mL chloroform) and the mixture stirred at room temperature. After 5 hours, the mixture was filtered over diatomaceous earth and the filtrate concentrated in vacuo. Purification of the resulting oil by flash chromatography on silica gel (hexane:ethyl acetate, 95:5; then 90:10) gave the title compound (2.26 g).
後処理
- filtrationthe mixture was filtered over diatomaceous earth
- concentrationthe filtrate concentrated in vacuo
- customPurification of the resulting oil by flash chromatography on silica gel (hexane
出典と根拠
- ORDレコード
- ord-24acdfef56a14e40b320a0f8063888a5
- 出典データセット
- uspto-grants-2000_11
- 特許番号
- US06150352
反応ノート
読み込み中…