반응 #629394

반응 방정식

Phosphorous oxychloride

dimethylacetamide

2-cyano-4,5-dimethoxyaniline

→

N,N-dimethyl-N'-(2-cyano-4,5-dimethoxyphenyl)acetamidine

용매

chloroform

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction stirred
2. 2
   온도under reflux for 4 hours
3. 3
   온도The mixture was cooled
4. 4
   workup.ADDITIONpoured onto ice
5. 5
   추출extracted with chloroform
6. 6
   추출extracted with chloroform
7. 7
   세척the combined extracts washed with water
8. 8
   건조dried (Na2SO4)
9. 9
   기타evaporated in vacuo
10. 10
    기타A sample of the brown oily residue (2 g) was crystallised from diisopropylether

실험 절차

Phosphorous oxychloride (1.0 ml) was added to a stirred solution of dimethylacetamide (2.8 ml) in chloroform (10 ml) at room temperature. The mixture was stirred for 5 minutes, 2-cyano-4,5-dimethoxyaniline (1.78 g) added and the reaction stirred under reflux for 4 hours. The mixture was cooled, poured onto ice and extracted with chloroform and the organic phase discarded. The aqueous layer was basified (solid NaOH) extracted with chloroform, the combined extracts washed with water, dried (Na2SO4) and evaporated in vacuo. A sample of the brown oily residue (2 g) was crystallised from diisopropylether to give N,N-dimethyl-N'-(2-cyano-4,5-dimethoxyphenyl)acetamidine, m.p. 94°-96°.

출처