تفاعل #1354117

معادلة التفاعل

3-(N,N-diethlyamino)phenol

3-chloro-2-hydrazino-5-trifluoromethylpyridine

hydrogen peroxide water

iodine

→

2-(3-chloro-5-trifluoromethyl-2-pyridylazo)-5-(diethylamino)phenol

المذيبات

Water

acetic acid

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere mixed
2. 2
   workup.STIRRINGthe mixture was stirred overnight
3. 3
   استخلاصfollowed by extraction with ether
4. 4
   أخرىcondensed
5. 5
   أخرىto precipitate crystals
6. 6
   ترشيحThe crystals were filtrated for collection
7. 7
   أخرىdried
8. 8
   أخرىto give

الإجراء التجريبي

Next, a reaction flask was loaded with 3-(N,N-diethlyamino)phenol (1.3 g), dimethylformamide (9 ml), acetic acid (3 ml) and iodine (0.14 g), and they were mixed, followed by addition of 3-chloro-2-hydrazino-5-trifluoromethylpyridine (1.0 g) to the flask with stirring. Then, to this mixture, a 30 % hydrogen peroxide water (1.4 g) was dropwise added in one hour and the mixture was stirred overnight. Water was added to this reaction mixture, followed by extraction with ether. The organic layer was condensed to precipitate crystals. The crystals were filtrated for collection and dried to give intended crystals (0.5 g).

المصدر