Iodine chloride → HCID 57423920、化合物
反応式
[F:1][CH:2]([F:11])[O:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][CH:10]=1)[NH2:7].[I:12]Cl.C([O-])(=O)C.[Na+]>C(O)(=O)C>[F:1][CH:2]([F:11])[O:3][C:4]1[CH:10]=[CH:9][C:8]([I:12])=[C:6]([CH:5]=1)[NH2:7]参加物
5
実験手順
A solution of 3-[(difluoromethyl)oxy]aniline (3.16 g), iodine monochloride (3.9 g) and sodium acetate (6.5 g) in acetic acid (30 ml) was stirred for 1 hour, then partitioned between saturated sodium bicarbonate solution and ether. The ether layer was separated, washed consecutively with sodium thiosulphate solution and brine. The solvent was removed and the residue was loaded onto a silica gel and chromatographed on silica gel eluted with hexane/ethyl acetate 0-20% to give the title compound as a red oil (2.9 g). Mass Spectrum 286 M+H+
後処理
- custompartitioned between saturated sodium bicarbonate solution and ether
- customThe ether layer was separated
- washwashed consecutively with sodium thiosulphate solution and brine
- customThe solvent was removed
- customchromatographed on silica gel
- washeluted with hexane/ethyl acetate 0-20%
出典と根拠
- ORDレコード
- ord-6dd9bd3588d94237b761d4931977ed46
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08288413B2
反応ノート
読み込み中…