반응 #86445

반응 방정식

1-ethyl-piperazine

5-fluoro-2-nitro-phenylamine

DIPEA

→

title compound

수율 63.0%

5-(4-Ethyl-piperazin-1-yl)-2-nitro-phenylamine

수율 63.0%

용매

DMF

반응 조건

후처리

1. 1
   추출extracted with EtOAc
2. 2
   추출The combined extract
3. 3
   세척was washed with brine
4. 4
   건조dried over anhydrous Na2SO4
5. 5
   농축concentrated
6. 6
   기타to obtain a crude product, which
7. 7
   기타was purified by flash chromatography on silica

실험 절차

A mixture of 1-ethyl-piperazine (1.2 mL, 9.6 mmol), 5-fluoro-2-nitro-phenylamine (1 g, 6.4 mmol), DIPEA (1.24 g, 9.6 mmol) in DMF (15 mL) was heated at 80° C. overnight. The reaction mixture was poured into ice water and extracted with EtOAc. The combined extract was washed with brine, dried over anhydrous Na2SO4, and concentrated to obtain a crude product, which was purified by flash chromatography on silica to afford the title compound (1 g, yield: 63%). ESI-MS: 251 [M+H]+.

출처