تفاعل #1584850

معادلة التفاعل

CDI

3-fluoro-pyridine-2-carboxylic acid

ethyl potassium malonate

MgCl2

→

3-(3-Fluoro-pyridin-2-yl)-3-oxo-propionic acid ethyl ester

المذيبات

water

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled to room temperature
2. 2
   workup.STIRRINGThe mixture was stirred at room temperature for 1 h
3. 3
   workup.ADDITIONthis reaction mixture was then added to the above suspension
4. 4
   workup.STIRRINGstirred at room temperature for 18 h
5. 5
   workup.ADDITIONwas added
6. 6
   استخلاصthe mixture was extracted with ethyl acetate
7. 7
   غسيلThe organic layer was washed with brine
8. 8
   تجفيفdried over Na2SO4
9. 9
   تركيزconcentrated

الإجراء التجريبي

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.

المصدر