反応 #158274

反応方程式

HATU

5-chloro-2-(4-chlorophenyl)-2-methylpentanoic acid

3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzohydrazide

triethylamine

→

title compound

収率 82.6%

N′-[5-chloro-2-(4-chlorophenyl)-2-methylpentanoyl]-3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzohydrazide

収率 82.6%

溶媒

ethyl acetate

water

brine

DMF

反応条件

後処理

1. 1
   抽出the mixture was extracted with ethyl acetate
2. 2
   洗浄The extract was washed with saturated brine (4×50 mL)
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   その他the solvent was evaporated under reduced pressure
5. 5
   その他The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

実験手順

To a mixture of 5-chloro-2-(4-chlorophenyl)-2-methylpentanoic acid (6.34 g), 3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzohydrazide (5.0 g) and triethylamine (6.78 mL) in DMF (50 mL) was added HATU (9.23 g) at 0° C., and the mixture was stirred at room temperature for 14 hr. The reaction mixture was diluted with ethyl acetate (50 mL), water (150 mL) and saturated brine (50 mL), and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine (4×50 mL), and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (8.19 g).

出典