反応 #453498

反応方程式

N,N-dimethylformamide

3-(4-chloro-2-ethyl-6-fluorobenzofuran-7-yl)-6-trifluoromethyluracil

2,4-dinitrophenoxyamine

potassium carbonate

→

desired product

収率 58.0%

3-(4-chloro-2-ethyl-6-fluorobenzofuran-7-yl)-1-amino-6-trifluoromethyluracil

収率 58.0%

溶媒

water

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   抽出extracted with ethyl acetate
3. 3
   洗浄The organic layer was washed sequentially with water
4. 4
   乾燥a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
6. 6
   その他Then, the obtained residue was purified by silica gel column chromatography

実験手順

80 ml of N,N-dimethylformamide was added to 3.4 g (9.0 mmol) of 3-(4-chloro-2-ethyl-6-fluorobenzofuran-7-yl)-6-trifluoromethyluracil, 2.7 g (14 mmol) of 2,4-dinitrophenoxyamine and 5.0 g (36 mmol) of potassium carbonate, followed by stirring at 60 to 70° C. for 1 hour. After completion of the reaction, the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed sequentially with water and a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 2.0 g (yield: 58%) of the desired product as white crystals. Melting point: 145-147° C.

出典