Tetrahydrofuran → HCID 58273767、化合物

HRID 2093126ノート

反応式

HRID 2093126 の反応式
[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

7

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

  1. customto this, a suspension formed
  2. additionwas added dropwise
  3. temperatureThereafter, the solution was heated to 90° C.
  4. stirringstirred for 9 hours
  5. customto separate the organic layer
  6. washThe organic layer was washed with 300 ml of water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationThe resulting solution was concentrated by a rotary evaporator
  9. 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

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