Methanol → Methyl 4-bromo-2-(methylsulfonyl)benzoate
反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:3]=1.S(=O)(=O)(O)O.[CH3:20]O>>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:20])=[O:7])=[C:4]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:3]=1参加物
4
実験手順
A suspension of 4-bromo-2-(methylsulphonyl)benzoic acid (5.00 g; 17.9 mmol) in MeOH (100 ml) was treated with conc. sulphuric acid and the resulting mixture was heated at reflux for 5 days. The mixture was concentrated under reduced pressure, the residue was dissolved in EtOAc then washed with water, twice with NaHCO3 (sat) then with brine, dried on MgSO4, filtered and concentrated to give the title compound as a yellow solid (4.00 g, 72%).
後処理
- temperaturethe resulting mixture was heated
- temperatureat reflux for 5 days
- concentrationThe mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in EtOAc
- washthen washed with water, twice with NaHCO3 (sat)
- dry with materialwith brine, dried on MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-10fee52c43184a85a00800637e46a4c6
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08273769B2
反応ノート
読み込み中…