反应 #45624

反应方程式

benzyloxyacetyl chloride

tetrahydrofuran

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

sodium hydrogencarbonate

→

compound

收率 77.2%

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

收率 77.2%

溶剂

Ethyl acetate

反应条件

后处理

1. 1
   温度cooled with ice
2. 2
   洗涤by washing with water and saturated brine
3. 3
   干燥The obtained organic layer was dried over anhydrous sodium sulfate
4. 4
   其他the solvent was evaporated away under reduced pressure
5. 5
   其他The resulting residue was recrystallized
6. 6
   其他purified with n-hexane/ethyl acetate

实验过程

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.

来源