反応 #45627

反応方程式

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

溶媒

ethyl acetate

反応条件

後処理

1. 1
   温度cooled with ice
2. 2
   workup.STIRRINGstirring at 60° C. for 1 hour
3. 3
   温度After cooling
4. 4
   洗浄by washing with water and saturated brine
5. 5
   乾燥The obtained organic layer was dried over anhydrous sodium sulfate
6. 6
   その他the solvent was evaporated away under reduced pressure

実験手順

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.

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