反应详情

温度

70 °C

1.46 ml of thionyl chloride (20 mmol) were added to a solution of 1.38 g of 3-(2-furyl)acrylic acid (10 mmol) in 10 ml of chloroform and 0.1 ml of DMF. The solution was warmed to 70° C. and kept at this temperature for 1 h, then the solvents were removed under reduced pressure and the residue was dissolved in 6.6 ml of DCM and 3.3 ml of pyridine and subsequently cooled to 0° C. 0.96 ml of 2-propanol (12.5 mmol) was added, the temperature was increased to RT and the reaction mixture was stirred for 2.5 h. It was acidified with 30 ml of 1 M hydrochloric acid and extracted with 150 ml of ethyl acetate. The organic phase was washed with aqueous sodium hydrogencarbonate solution, dried over sodium sulfate, filtered and the solvents were removed under reduced pressure. 1.72 g (yield: 96%) of the title compound were obtained. LC/MS (Method D) (M+H-isopropyl)+ 139

1. customthe solvents were removed under reduced pressure
2. dissolutionthe residue was dissolved in 6.6 ml of DCM
3. temperature3.3 ml of pyridine and subsequently cooled to 0° C
4. temperaturethe temperature was increased to RT
5. extractionextracted with 150 ml of ethyl acetate
6. washThe organic phase was washed with aqueous sodium hydrogencarbonate solution
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customthe solvents were removed under reduced pressure