반응 #45627

반응 방정식

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

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도cooled with ice
2. 2
   workup.STIRRINGstirring at 60° C. for 1 hour
3. 3
   온도After cooling
4. 4
   세척by washing with water and saturated brine
5. 5
   건조The obtained organic layer was dried over anhydrous sodium sulfate
6. 6
   기타the solvent was evaporated away under reduced pressure

실험 절차

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.

출처