Boron tribromide → 3-Amino-2-chloro-4-fluorophenol
反応式
[Cl:1][C:2]1[C:8]([O:9]C)=[CH:7][CH:6]=[C:5]([F:11])[C:3]=1[NH2:4].B(Br)(Br)Br.C([O-])(O)=O.[Na+]>C(Cl)Cl>[NH2:4][C:3]1[C:2]([Cl:1])=[C:8]([OH:9])[CH:7]=[CH:6][C:5]=1[F:11]参加物
5
実験手順
To a solution of 2-chloro-6-fluoro-3-methoxy-aniline (0.85 g, 4.84 mmol, 1.0 eq) in DCM (8 mL) at 0° C. was added BBr3 (6.06 g, 24.2 mmol, 5.0 eq). The mixture was stirred at room temperature under N2 overnight, then poured into ice-water. The pH of the solution was adjusted to pH 6 by addition of sat.NaHCO3. The dichloromethane was removed under reduced pressure and the aqueous residue was extracted with EtOAc. The combined organic extracts were washed with brine, dried (Na2SO4), filtered and evaporated in vacuo to give the title compound as a pale yellow solid (0.74 g, 95%).
後処理
- additionThe pH of the solution was adjusted to pH 6 by addition
- customThe dichloromethane was removed under reduced pressure
- extractionthe aqueous residue was extracted with EtOAc
- washThe combined organic extracts were washed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-75f2b7f7b4bd4bf2b7e379593e098b82
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09249085B2
反応ノート
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