反应详情

温度

75 °C

In 5 mL of dimethyl sulfoxide was dissolved 1.00 g of 6-[2-(3-chloropropoxy)ethyl]-1-benzothiophene, and 0.86 g of 3-azetidinol hydrochloride and 1.63 g of potassium carbonate were added to the solution. The resulting mixture was stirred at 75° C. for 2.5 hours and then at 95° C. for 1.5 hours. After the reaction mixture was cooled, water and ethyl acetate were added thereto and the pH was adjusted to 1 with 6 mol/L hydrochloric acid, and the aqueous layer was separated. Ethyl acetate was added to the aqueous layer and the. pH was adjusted to 10 with a 2 mol/L aqueous sodium hydroxide solution, after which the organic layer was separated. The organic layer was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by a column chromatography (eluent; chloroform:methanol=30:1 to 5:1) to obtain 0.28 g of 1-{3-[2-(1-benzothiophen-6-yl)ethoxy]propyl}-3-azetidinol as a colorless oil.

1. additionwere added to the solution
2. waitat 95° C. for 1.5 hours
3. temperatureAfter the reaction mixture was cooled
4. customthe aqueous layer was separated
5. additionEthyl acetate was added to the aqueous layer
6. customafter which the organic layer was separated
7. washThe organic layer was washed with water
8. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
9. distillationdistilled under reduced pressure
10. customto remove the solvent
11. customThe residue was purified by a column chromatography (eluent; chloroform:methanol=30:1 to 5:1)