Methanol → HCID 68502921、化合物
反応式
[CH3:1][C:2]1[C:10]2[O:9][C:8]([C:11]([OH:13])=[O:12])=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH3:14]O>OS(O)(=O)=O>[CH3:1][C:2]1[C:10]2[O:9][C:8]([C:11]([O:13][CH3:14])=[O:12])=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
A solution of 4.32 g of 7-methylbenzofuran-2-carboxylic acid in 150 ml of methanol and 1 ml of conc. H2SO4 is stirred at reflux over 9 hours. The reaction mixture is cooled and concentrated by evaporation. The residue is dissolved in diethyl ether and washed with water, saturated aqueous sodium hydrogencarbonate solution and brine, dried over sodium sulphate and concentrated by evaporation. The crude title compound is obtained as a red-brown oil from the residue. Rf=0.32 (1:6 EtOAc-heptane); Rt=4.51.
後処理
- temperatureat reflux over 9 hours
- temperatureThe reaction mixture is cooled
- concentrationconcentrated by evaporation
- dissolutionThe residue is dissolved in diethyl ether
- washwashed with water, saturated aqueous sodium hydrogencarbonate solution and brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated by evaporation
出典と根拠
- ORDレコード
- ord-1457b75f028c47ce852ebfebff9cae80
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07842688B2
反応ノート
読み込み中…