反应详情

6 ml of piperidine was stirred in dichloromethane at 0° C., and a solution of 3 g (15 mmol) of monomethyl terephthalate chloride in dichloromethane was added to the resultant mixture. The temperature was elevated to room temperature, and they were stirred for 2 hours and then diluted with 1 N hydrochloric acid. After the extraction with dichloromethane, the organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and then with saturated aqueous NaCl solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was stirred in ethanol. 30 ml of 1 N aqueous sodium hydroxide solution was added to the resultant mixture, and they were stirred at room temperature overnight. The solvent was evaporated, and the reaction liquid was concentrated and then diluted with 1 N hydrochloric acid. After the extraction with ethyl acetate, the organic layer was washed with saturated aqueous NaCl solution and dried over anhydrous magnesium sulfate. The solvent was evaporated to obtain the title compound.

1. customwas elevated to room temperature
2. extractionAfter the extraction with dichloromethane
3. washthe organic layer was washed with saturated aqueous sodium hydrogencarbonate solution
4. dry with materialwith saturated aqueous NaCl solution, and dried over anhydrous magnesium sulfate
5. customThe solvent was evaporated
6. stirringthe residue was stirred in ethanol
7. addition30 ml of 1 N aqueous sodium hydroxide solution was added to the resultant mixture, and they
8. stirringwere stirred at room temperature overnight
9. customThe solvent was evaporated
10. customthe reaction liquid
11. concentrationwas concentrated
12. additiondiluted with 1 N hydrochloric acid
13. extractionAfter the extraction with ethyl acetate
14. washthe organic layer was washed with saturated aqueous NaCl solution
15. dry with materialdried over anhydrous magnesium sulfate
16. customThe solvent was evaporated