تفاعل #45627

معادلة التفاعل

cinnamoyl chloride

tetrahydrofuran

2-amino-5-phenyl-4-fluoro-3-hydroxy-6-methylbenzonitrile

sodium hydrogencarbonate

→

(E)-N-(3-Cyano-6-fluoro-5-hydroxy-2-methyl[1,1′-biphenyl]-4-yl)-3-phenyl-2-propenamide

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled with ice
2. 2
   workup.STIRRINGstirring at 60° C. for 1 hour
3. 3
   درجة الحرارةAfter cooling
4. 4
   غسيلby washing with water and saturated brine
5. 5
   تجفيفThe obtained organic layer was dried over anhydrous sodium sulfate
6. 6
   أخرىthe solvent was evaporated away under reduced pressure

الإجراء التجريبي

Under nitrogen atmosphere, cinnamoyl chloride (378 mg, 2.27 mmol) was dropwise added to a tetrahydrofuran solution (10 ml) of 2-amino-5-phenyl-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-41) (500 mg, 2.06 mmol) and sodium hydrogencarbonate (399 mg, 4.75 mmol) cooled with ice, followed by stirring at room temperature for 17 hours and stirring at 60° C. for 1 hour. After cooling, ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine. The obtained organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure.

المصدر