Sodium Iodide → 1-Iodoethyl 2-acetoxybenzoate
反応式
CC1[O:7][CH:6]([CH3:8])[O:5][CH:4]([CH3:9])O1.[Na+].[I-:11].[C:12]([O:15][C:16]1C=[CH:20][CH:19]=[CH:18][C:17]=1C(Cl)=O)(=[O:14])[CH3:13]>C(Cl)Cl>[C:12]([O:15][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:8]=1[C:6]([O:5][CH:4]([I:11])[CH3:9])=[O:7])(=[O:14])[CH3:13]参加物
5
実験手順
To a mixture of 2,4,6-trimethyl-1,3,5-trioxane (245 mg, 1.85 mmol) and NaI (0.972 g, 6.48 mmol) in DCM (15 mL) was added a solution of 2-(chlorocarbonyl)-phenyl acetate in DCM (5 mL, 0° C.). The resulting mixture was allowed to stir (RT, 16 h). The mixture was filtrated and concentrated under reduced pressure. The crude was purified by silica gel chromatography (EtOAc-PE, 0-10%) to afford 1-iodoethyl 2-acetoxybenzoate (0.75 g, 40%) as a light yellow oil.
後処理
- filtrationThe mixture was filtrated
- concentrationconcentrated under reduced pressure
- customThe crude was purified by silica gel chromatography (EtOAc-PE, 0-10%)
出典と根拠
- ORDレコード
- ord-72a7ffef402a44e3a4b4c7489ec3f10c
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846972B2
反応ノート
読み込み中…