تفاعل #1354119

معادلة التفاعل

3-(N,N-diethylamino)phenol

3,5-dichloro-2-hydrazinopyridine

hydrogen peroxide water

iodine

→

2-(3,5-dichloro-2-pyridylazo)-5-(diethylamino)phenol

المذيبات

acetic acid

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere mixed
2. 2
   workup.STIRRINGthe mixture was stirred overnight
3. 3
   ترشيحThe reaction mixture was filtrated
4. 4
   workup.ADDITIONether and water were added to the filtrate
5. 5
   workup.STIRRINGby stirring
6. 6
   workup.STIRRINGAfter stirring
7. 7
   أخرىthe ether layer was collected
8. 8
   أخرىcondensed
9. 9
   أخرىto precipitate crystals
10. 10
    ترشيحThe crystals were filtrated for collection
11. 11
    أخرىdried
12. 12
    أخرىto give

الإجراء التجريبي

Next, a flask was loaded with 3-(N,N-diethylamino)phenol (1.7 g), dimethylformamide (14 ml), acetic acid (5 ml) and iodine (0.24 g), and they were mixed, followed by addition of 3,5-dichloro-2-hydrazinopyridine (1.6 g) to the flask with stirring. Then, to this, a 30% hydrogen peroxide water (2.4 g) was dropwise added in 90 minutes and the mixture was stirred overnight. The reaction mixture was filtrated, and ether and water were added to the filtrate, followed by stirring. After stirring, the ether layer was collected and condensed to precipitate crystals. The crystals were filtrated for collection and dried to give intended crystals (0.54 g).

المصدر