Sodium Iodide → 2-Iodo-4-(trifluoromethyl)phenol
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[Na+].[I-:13]>CN(C=O)C.Cl>[I:13][C:5]1[CH:4]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:8]=[CH:7][C:6]=1[OH:9]参加物
5
実験手順
4-(trifluoromethyl)-phenol (8 g) in anhydrous DMF (80 ml) was cooled to 0° C. NaI (9.06 g) and chloroamine-T (16.1 g) was added portionwise and stirred at room temperature overnight. Then diluted with 2M HCl and extracted with ethylacetate. The organic phase was washed with sodium thiosulfate solution, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography (silica, eluting with isohexane:ethyl acetate) to give the sub-title compound as a yellow oil (13 g).
後処理
- extractionextracted with ethylacetate
- washThe organic phase was washed with sodium thiosulfate solution
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography (silica, eluting with isohexane:ethyl acetate)
出典と根拠
- ORDレコード
- ord-1e2552f608414f098ff5e79320e33a6d
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737135B2
反応ノート
読み込み中…