반응 #1095077

ord-96b64a41c607495883c81ef1f8893c3b

반응 방정식

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

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The organic layer is separated
  2. 2
    세척washed with water and saturated aqueous solution of sodium chloride
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure
  5. 5
    기타the residue is purified by column chromatography (eluent: chloroform:methanol=10:1)

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06797726B1uspto-grants-2004_09