反应 #1354119

反应方程式

3-(N,N-diethylamino)phenol

3,5-dichloro-2-hydrazinopyridine

hydrogen peroxide water

iodine

→

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

溶剂

acetic acid

dimethylformamide

反应条件

后处理

1. 1
   workup.ADDITIONwere mixed
2. 2
   workup.STIRRINGthe mixture was stirred overnight
3. 3
   过滤The 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
   其他the ether layer was collected
8. 8
   其他condensed
9. 9
   其他to precipitate crystals
10. 10
    过滤The crystals were filtrated for collection
11. 11
    其他dried
12. 12
    其他to give

实验过程

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).

来源