Tetrahydrofuran → HCID 58273767、化合物
反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH2:7][OH:8].[H-].[Na+].O1CCCC1.Br[CH2:17][CH2:18][O:19][CH2:20][CH2:21][CH2:22][CH3:23]>CCCCCC.O>[CH2:20]([O:19][CH2:18][CH2:17][O:8][CH2:7][CH2:6][C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)[CH2:21][CH2:22][CH3:23]参加物
反応条件
- 温度
- 0 °C
実験手順
6.1 g of 2-thiopheneethanol was cooled to 0° C., and to this, a suspension formed by adding 2.8 g of sodium hydride (60% in oil) to 50 ml of tetrahydrofuran was added dropwise. The solution was stirred at 0° C. for 20 minutes under a nitrogen atmosphere, and to this, 8.2 g of 1-(2-bromo-ethoxy)-butane was added dropwise. Thereafter, the solution was heated to 90° C. and stirred for 9 hours. 100 ml of water and 100 ml of hexane were added to the reaction solution to separate the organic layer. The organic layer was washed with 300 ml of water and then dried over anhydrous magnesium sulfate. The resulting solution was concentrated by a rotary evaporator and purified by a column chromatography (filler: silica gel, eluent: hexane/dichloromethane) to obtain 3.5 g of 2-[2-(2-butoxy-ethoxy)ethyl]-thiophene.
後処理
- customto this, a suspension formed
- additionwas added dropwise
- temperatureThereafter, the solution was heated to 90° C.
- stirringstirred for 9 hours
- customto separate the organic layer
- washThe organic layer was washed with 300 ml of water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationThe resulting solution was concentrated by a rotary evaporator
- custompurified by a column chromatography (filler: silica gel, eluent: hexane/dichloromethane)
出典と根拠
- ORDレコード
- ord-a73e88e80135411d86ba75235f95c86e
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08441002B2
反応ノート
読み込み中…