Sodium Iodide → HCID 9999073、化合物
反応式
CS(O[CH2:6][CH:7]1[O:12][C:11]2[CH:13]=[C:14]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:15]=[CH:16][C:10]=2[O:9][CH2:8]1)(=O)=O.[I-:24].[Na+]>C(C(C)=O)C.C(OCC)(=O)C>[I:24][CH2:6][CH:7]1[O:12][C:11]2[CH:13]=[C:14]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:15]=[CH:16][C:10]=2[O:9][CH2:8]1参加物
5
実験手順
2-Methanesulfonyloxymethyl-7-phenoxy-1,4-benzodioxane (1.85 g, 5.5 mmol) and sodium iodide (1.54 g, 11.0 mmol) are taken up in methyl ethyl ketone (60 mL) and heated at reflux for 3 hours. The mixture is cooled, diluted with ethyl acetate, washed with aqueous sodium bicarbonate, dried over magnesium sulfate and evaporated to give 2-iodomethyl-7-phenoxy-1,4-benzodioxane as a tan solid. This is used without further purification.
後処理
- temperatureheated
- temperatureat reflux for 3 hours
- temperatureThe mixture is cooled
- washwashed with aqueous sodium bicarbonate
- dry with materialdried over magnesium sulfate
- customevaporated
出典と根拠
- ORDレコード
- ord-5e011c08835541709630206838ac3f12
- 出典データセット
- uspto-grants-1992_06
- 特許番号
- US05120758
反応ノート
読み込み中…