Iodine chloride → HCID 57423920, 화합물
반응식
[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]참가 물질
5
실험 절차
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+
후처리
- 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%
출처 및 근거
- ORD 기록
- ord-6dd9bd3588d94237b761d4931977ed46
- 출처 데이터셋
- uspto-grants-2012_10
- 특허 번호
- US08288413B2
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