تفاعل #671002

معادلة التفاعل

4-mercaptopyridine

3,4-difluoro-nitrobenzene

potassium carbonate

→

4-[(2-Fluoro-4-nitrophenyl)sulphanyl]pyridine

المذيبات

ethyl acetate

water

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe aqueous phase is extracted five times with in each case 100 mL of ethyl acetate
2. 2
   غسيلThe combined organic phases are washed with 200 mL of saturated sodium chloride solution
3. 3
   تجفيفdried over sodium sulphate
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   أخرىa rotary evaporator
6. 6
   أخرىThe residue is purified by MPLC (mobile phase: ethyl acetate:cyclohexane 1:1)

الإجراء التجريبي

21 g (188.9 mmol) of 4-mercaptopyridine, 30.05 g (188.9 mmol) of 3,4-difluoro-nitrobenzene and 60.05 g (434.5 mmol) of potassium carbonate are dissolved in dimethylformamide, and the mixture is stirred at 40° C. for 3 hours. The reaction solution is then diluted with 500 mL of ethyl acetate and 300 mL of water. The aqueous phase is extracted five times with in each case 100 mL of ethyl acetate. The combined organic phases are washed with 200 mL of saturated sodium chloride solution, dried over sodium sulphate and concentrated under reduced pressure using a rotary evaporator. The residue is purified by MPLC (mobile phase: ethyl acetate:cyclohexane 1:1).

المصدر