1,1'-Carbonyldiimidazole → Ethyl 3-(3-fluoropyridin-2-yl)-3-oxopropanoate

温度

50 °C

To a solution of ethyl potassium malonate (2) (452 mg, 2.66 mmol) in tetrahydrofuran (5 mL) was added MgCl2 (202 mg, 2.13 mL). The mixture was stirred at 50° C. for 4 h and then cooled to room temperature. In another flask a solution of 3-fluoro-pyridine-2-carboxylic acid (1) (250 mg, 1.77 mmol) in tetrahydrofuran (5 mL) was taken and CDI (carbonyldiimidazole) (489 mg, 3.01 mmol) was added at 10° C. The mixture was stirred at room temperature for 1 h, this reaction mixture was then added to the above suspension and stirred at room temperature for 18 h. After completion of the reaction, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over Na2SO4 and concentrated.

1. temperaturecooled to room temperature
2. stirringThe mixture was stirred at room temperature for 1 h
3. additionthis reaction mixture was then added to the above suspension
4. stirringstirred at room temperature for 18 h
5. additionwas added
6. extractionthe mixture was extracted with ethyl acetate
7. washThe organic layer was washed with brine
8. dry with materialdried over Na2SO4
9. concentrationconcentrated

ORDレコード

ord-0fbbb22fccd4481b8eaf2fb12366883b

出典データセット

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09199987B2