Phenyl acetamide derivative
A technology of phenylacetamide and derivatives, which is applied in the field of new phenylacetamide derivatives and can solve problems such as unspecified compounds
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manufacture example 1
[0216] To a 60% solution of sodium hydride (496 mg) in DMF (10 mL) was added a solution of 1H-pyrazol-3-amine (1.03 g) in DMF (5 mL) under ice-cooling and stirred at room temperature for 30 minutes. A solution of [(3-bromopropoxy)methyl]benzene (2.93 g) in DMF (10 mL) was added under ice-cooling, followed by stirring at room temperature overnight. Saturated saline and saturated aqueous sodium bicarbonate solution were added, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The obtained crude product was purified by silica gel column chromatography (hexane:ethyl acetate=1:1-1:3) to obtain 1-[3-(benzyloxy)propyl]-1H as a pale yellow oil - Pyrazol-3-amine (835 mg).
manufacture example 2
[0218] Add bromocyclopropane (41.6g), potassium carbonate (54.8g) and triphenylmethanethiol (1.46g) in the DMF (500mL) solution of 2-bromothiophenol (50g), and internal temperature 80 Stir at °C for 24 hours. After cooling to room temperature, water and ethyl acetate were added, and the organic layer was separated. The organic layer was washed with saturated aqueous sodium bicarbonate and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 1-bromo-2-(cyclopropylthio)benzene (49.3 g).
manufacture example 3
[0220] To a suspension of aluminum chloride (40.2 g) in dichloromethane (1200 mL) was added dropwise ethyl chloro(oxo)acetate (32.3 g) at 0°C, followed by stirring at the same temperature for 1 hour. A dichloromethane (280 mL) solution of 1-bromo-2-(cyclopropylthio)benzene (49.3 g) was added dropwise while keeping the reaction liquid below 5° C., and stirred at room temperature for 1 hour. The reaction solution was cooled to 0°C, and water was added to stop the reaction. The reaction solution was extracted with ethyl acetate, and the organic layer was washed successively with water, saturated aqueous sodium bicarbonate solution and saturated brine. After drying over anhydrous magnesium sulfate, it was concentrated. The residue was purified by silica gel column chromatography to obtain ethyl [3-bromo-4-(cyclopropylthio)phenyl](oxo)acetate (29.8 g).
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