تفاعل #81869

معادلة التفاعل

HNO3

NaOH

H2SO4

2-amino-5-chloropyridine

→

2

المردود 56.0%

2-Amino-5-chloro-3-nitropyridine

المردود 56.0%

المذيبات

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthat maintain the temperature within 50°-55° C.) over 1 h
2. 2
   workup.STIRRINGThe resulting mixture was stirred at 60° C. for 3 h
3. 3
   workup.STIRRINGwith stirring
4. 4
   workup.STIRRINGwith stirring
5. 5
   درجة الحرارةcooling
6. 6
   ترشيحThe precipitate was filtered
7. 7
   غسيلwashed with water (6×50 mL)
8. 8
   أخرىdried

الإجراء التجريبي

To 150 mL of conc. H2SO4 was added 42.96 g (334 mmol) of 2-amino-5-chloropyridine in portions with stirring and cooling (ice-water bath). To the resulting solution was added dropwise 22.5 mL of 69-71% HNO3 (355 mmol) at 50° C. (at such a rate that maintain the temperature within 50°-55° C.) over 1 h. The resulting mixture was stirred at 60° C. for 3 h, poured into ice-water (about 1,500 mL) with stirring, then basified to pH 9 by the addition of 40% aq NaOH with stirring and cooling. The precipitate was filtered, washed with water (6×50 mL), and dried to give 32.47 g (56%) of 2 as a yellow powder, mp 190°-191° C. (lit. 191°-2° C. (Israel, M. & Day, A. R., J. Org. Chem. 24:1455-1460 (1959))). 1H NMR (DMSO-d6), 8.044-8.055 (m, 3H), 8.054 (d, 1H, J=3.9).

المصدر