تفاعل #45624

معادلة التفاعل

benzyloxyacetyl chloride

tetrahydrofuran

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

sodium hydrogencarbonate

→

compound

المردود 77.2%

2-(Benzyloxy)-N-(3-cyano-6-fluoro-5-hydroxy-2-methyl[1,1′-biphenyl]-4-yl)acetamide

المردود 77.2%

المذيبات

Ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled with ice
2. 2
   غسيلby washing with water and saturated brine
3. 3
   تجفيفThe obtained organic layer was dried over anhydrous sodium sulfate
4. 4
   أخرىthe solvent was evaporated away under reduced pressure
5. 5
   أخرىThe resulting residue was recrystallized
6. 6
   أخرىpurified with n-hexane/ethyl acetate

الإجراء التجريبي

Under nitrogen atmosphere, benzyloxyacetyl chloride (489 μl, 3.10 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 (520 mg, 6.19 mmol) cooled with ice, followed by stirring at room temperature for 18 hours. 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. The resulting residue was recrystallized and purified with n-hexane/ethyl acetate to obtain the entitled compound (621 mg, 1.59 mmol, 77%) as a white solid.

المصدر