반응 #41803

반응 방정식

benzyl alcohol

2-Fluoro-3-(4-methyl-piperazin-1-yl)-6-nitro-phenylamine

→

2

수율 94.4%

3-Fluoro-4-(4-methyl-piperazin-1-yl)-benzene-1,2-diamine

수율 94.4%

용매

EtOAc

반응 조건

후처리

1. 1
   기타A 250 mL reaction tube
2. 2
   기타The reaction tube was sealed
3. 3
   온도to cool to rt
4. 4
   여과filtered through Celite
5. 5
   세척washed successively with EtOAc, MeOH, and EtOH
6. 6
   농축The combine organics were concentrated

실험 절차

A 250 mL reaction tube was charged with benzyl alcohol 1 (1.0 g, 3.6 mmol), MnO2 (4.7 g, 54 mmol) and EtOAc (20 mL). The reaction tube was sealed was heated to 120° C. with stirring for 2 h. The reaction was allowed to cool to rt, then filtered through Celite and washed successively with EtOAc, MeOH, and EtOH. The combine organics were concentrated to give 936 mg (3.4 mmol, 94%) of 2 as an orange solid: 1H NMR (300 MHz, CDCl3) δ 10.01 (s, 1H), 8.64 (d, J=5.5 Hz, 1H), 8.09 (br s, 1H), 7.96 (d, J=2.75 Hz, 1H), 7.37 (d, J=2.48 Hz, 1H), 7.29 (d, J=2.75 Hz, 1H), 7.08 (dd, J=2.47, 5.5 Hz, 1H), 6.94 (d, J=9.35 Hz, 1H), 3.08 (d, J=5.23 Hz, 3H).

출처