반응 #76463

반응 방정식

water

1-chloro-3-iodopropane

1,2-dimethylphenothiazine

sodium hydride

→

title compound

수율 57.2%

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

수율 57.2%

용매

N,N′-dimethylformamide

반응 조건

후처리

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

실험 절차

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.

출처