반응 #453498

반응 방정식

N,N-dimethylformamide

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

2,4-dinitrophenoxyamine

potassium carbonate

→

desired product

수율 58.0%

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

수율 58.0%

용매

water

반응 조건

후처리

1. 1
   기타After completion of the reaction
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The organic layer was washed sequentially with water
4. 4
   건조a 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
   기타Then, the obtained residue was purified by silica gel column chromatography

실험 절차

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.

출처