Dimethyl Sulfate → 1-Bromo-3-tert-butyl-5-iodo-2-methoxybenzene
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-23e3c48b49ab4c73be74f1ebf34a802a
- 출처 데이터셋
- uspto-grants-2014_06
- 특허 번호
- US08748443B2
반응 노트
불러오는 중…