Reaktion #76463

Reaktionsgleichung

water

1-chloro-3-iodopropane

1,2-dimethylphenothiazine

sodium hydride

→

title compound

Ausbeute 57.2%

1,2-Dimethl-10-(3-chloropropyl)phenothiazine

Ausbeute 57.2%

Lösungsmittel

N,N′-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter stirring at room temperature for 30 min
2. 2
   workup.STIRRINGby stirring at room temperature overnight
3. 3
   Extraktionthe reaction mixture was extracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed with water
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   SonstigeAfter evaporating the solvent under reduced pressure
7. 7
   Sonstigethe residue was purified by silica gel column chromatography

Vorschrift

To a solution of 5.0 g of 1,2-dimethylphenothiazine in N,N′-dimethylformamide was added 970 mg of sodium hydride under stirring at room temperature. After stirring at room temperature for 30 min, 4.0 g of 1-chloro-3-iodopropane was added dropwise followed by stirring at room temperature overnight. After adding water, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. After evaporating the solvent under reduced pressure, the residue was purified by silica gel column chromatography to give 3.4 g of the title compound.

Quelle