تفاعل #86485

معادلة التفاعل

NaOH

HNO3

H2SO4

1-(4-fluorophenyl)ethanamine

→

title compound

المردود 98.0%

1-(4-fluoro-3-nitrophenyl)ethanamine

المردود 98.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwith cooling for 50 minutes
2. 2
   استخلاصThe alkaline solution was extracted with DCM twice
3. 3
   تجفيفThe combined organic layer was dried over Na2SO4
4. 4
   أخرىevaporated

الإجراء التجريبي

Fuming HNO3 (0.48 ml, 10.8 mmol) was added carefully to ice bath cooled concentrated H2SO4 (3.6 ml, 68.2 mmol). To the mixture was added 1-(4-fluorophenyl)ethanamine (1.0 g, 7.2 mmol) dropwise. The reaction mixture was stirred with cooling for 50 minutes. The reaction mixture was poured into ice and basified with 3M NaOH solution (24 ml, 72.00 mmol) to about pH8.0. The alkaline solution was extracted with DCM twice. The combined organic layer was dried over Na2SO4 and evaporated to afford title compound (1.3 g, yield: 96%). 1H-NMR (400 MHz, CDCl3) δ 1.41 (d, 6H) 4.25 (q, 1H) 7.21-7.26 (m, 1H) 7.67 (ddd, 1H) 8.10 (dd, 1H)

المصدر