反应详情

温度

100 °C

In 6 mL of N,N-dimethylformamide is dissolved 0.80 g of 5-[2-(3-chloropropyloxy)ethyl]benzo[b]-thiophene, to which is added 3.2 mL of diethylamine. The mixture is stirred in an ampoule at 100° C. for 10 hours. After cooling, the reaction mixture is introduced into a mixture of water and ethyl acetate, pH is adjusted to 1.0 with 6 mol/L hydrochloric acid, and the aqueous layer is separated. Ethyl acetate is added to the aqueous layer, pH is adjusted to 10.0 with 5 mol/L aqueous solution of sodium hydroxide, and the organic layer is separated. The organic layer is 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 to 4:1). Thus, 0.48 g of N-[3-(2-benzo[b]thiophen-5-ylethoxy)propyl]-N,N-diethylamine is obtained as an oily product.

1. temperatureAfter cooling
2. customthe aqueous layer is separated
3. additionEthyl acetate is added to the aqueous layer
4. customthe organic layer is separated
5. washThe organic layer is washed with water and saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationthe solvent is distilled off under reduced pressure
8. customthe residue is purified by column chromatography (eluent: chloroform:methanol=10:1 to 4:1)