Reaktion #1354117

Reaktionsgleichung

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

Lösungsmittel

Water

acetic acid

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere mixed
2. 2
   workup.STIRRINGthe mixture was stirred overnight
3. 3
   Extraktionfollowed by extraction with ether
4. 4
   Sonstigecondensed
5. 5
   Sonstigeto precipitate crystals
6. 6
   FiltrationThe crystals were filtrated for collection
7. 7
   Sonstigedried
8. 8
   Sonstigeto give

Vorschrift

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).

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