反応 #1095077

ord-96b64a41c607495883c81ef1f8893c3b

反応方程式

ClCCCOCCc1ccc2sccc2c1
5-[2-(3-chloropropyloxy)ethyl]benzo[b]-thiophene
CNCCO
2-(methylamino)ethanol
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O
water
CN(CCO)CCCOCCc1ccc2sccc2c1
2-{[3-(2-benzo[b]thiophen-5-ylethoxy)propyl]-(methyl)amino]-1-ethanol

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The organic layer is separated
  2. 2
    洗浄washed with water and saturated aqueous solution of sodium chloride
  3. 3
    乾燥dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure
  5. 5
    その他the residue is purified by column chromatography (eluent: chloroform:methanol=10:1)

実験手順

In 6 mL of N,N-dimethylformamide is dissolved 0.80 g of 5-[2-(3-chloropropyloxy)ethyl]benzo[b]-thiophene, to which are added 0.51 mL of 2-(methylamino)ethanol and 0.87 g of potassium carbonate. The mixture is stirred at 80° C. for 3 hours. The reaction mixture is introduced into a mixture of water and ethyl acetate. The organic layer is separated, washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, the solvent is distilled off under reduced pressure, and the residue is purified by column chromatography (eluent: chloroform:methanol=10:1). Thus, 0.59 g of 2-{[3-(2-benzo[b]thiophen-5-ylethoxy)propyl]-(methyl)amino]-1-ethanol is obtained as an oily product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06797726B1uspto-grants-2004_09