Reaktion #791499

Reaktionsgleichung

ethyl acetate

4-(5 chloro-2-pyrimidinyloxy)-3methylaniline

triethylamine

2-nitrobenzenesulfenyl chloride

→

N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide

Ausbeute 83.6%

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas dropwise added
2. 2
   Sonstigeat room temperature
3. 3
   SonstigeThe mixture was reacted at room temperature for 1 hour
4. 4
   workup.ADDITIONwas added to the reaction product
5. 5
   Waschenthe ethyl acetate layer was washed with water
6. 6
   Trocknendried over Glauber's salt
7. 7
   Sonstigepurified by column chromatography

Vorschrift

2.0 g of 4-(5 chloro-2-pyrimidinyloxy)-3methylaniline and 0.94 g of triethylamine were dissolved in 20 ml of toluene, and a solution of 1.61 g of 2-nitrobenzenesulfenyl chloride dissolved in 5 ml of toluene was dropwise added thereto at room temperature. The mixture was reacted at room temperature for 1 hour under stirring. After completion of the reaction, ethyl acetate was added to the reaction product, and the ethyl acetate layer was washed with water, dried over Glauber's salt and then purified by column chromatography to obtain 2.76 g of N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]-2-nitrobenzenesulfenamide (Intermediate Compound No. 37) (melting point: 74°-85° C.) in a yellow non-crystalline form.

Quelle