تفاعل #41803

معادلة التفاعل

benzyl alcohol

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

→

2

المردود 94.4%

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

المردود 94.4%

المذيبات

EtOAc

ظروف التفاعل

المعالجة

1. 1
   أخرىA 250 mL reaction tube
2. 2
   أخرىThe reaction tube was sealed
3. 3
   درجة الحرارةto cool to rt
4. 4
   ترشيحfiltered through Celite
5. 5
   غسيلwashed successively with EtOAc, MeOH, and EtOH
6. 6
   تركيزThe combine organics were concentrated

الإجراء التجريبي

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).

المصدر