Dimethyl Sulfate → 1-Bromo-3-tert-butyl-5-iodo-2-methoxybenzene
反応式
[Br:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:3]=1[OH:13].[C:14](=O)([O-])[O-].[K+].[K+].COS(OC)(=O)=O>CC(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[C:4]([C:9]([CH3:10])([CH3:12])[CH3:11])[C:3]=1[O:13][CH3:14]参加物
5
実験手順
A solution of 2-bromo-6-tert-butyl-4-iodophenol (5.0 g, 14.08 mmol) in acetone (50 mL) was treated with potassium carbonate (2.92 g, 21.13 mmol) and dimethylsulfate (1.95 g, 15.49 mmol) at reflux for 16 hours, cooled and concentrated. The residue was dissolved in ethyl acetate, washed with water, brine, dried (Na2SO4), filtered and concentrated in vacuo. The crude product was purified on an Isco 40 g silica cartridge eluting with 2% ethyl acetate in hexane to give the title compound.
後処理
- temperatureat reflux for 16 hours
- temperaturecooled
- concentrationconcentrated
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with water, brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude product was purified on an Isco 40 g silica cartridge
- washeluting with 2% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-23e3c48b49ab4c73be74f1ebf34a802a
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08748443B2
反応ノート
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