反応 #41803

反応方程式

benzyl alcohol

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

→

2

収率 94.4%

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

収率 94.4%

溶媒

EtOAc

反応条件

後処理

1. 1
   その他A 250 mL reaction tube
2. 2
   その他The reaction tube was sealed
3. 3
   温度to cool to rt
4. 4
   ろ過filtered through Celite
5. 5
   洗浄washed successively with EtOAc, MeOH, and EtOH
6. 6
   濃縮The combine organics were concentrated

実験手順

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).

出典