反应 #41803

反应方程式

benzyl alcohol

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

→

2

收率 94.4%

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

收率 94.4%

溶剂

EtOAc

反应条件

后处理

1. 1
   其他A 250 mL reaction tube
2. 2
   其他The reaction tube was sealed
3. 3
   温度to cool to rt
4. 4
   过滤filtered through Celite
5. 5
   洗涤washed successively with EtOAc, MeOH, and EtOH
6. 6
   浓缩The combine organics were concentrated

实验过程

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).

来源