반응 #42509

반응 방정식

2-chloro-6-methylisonicotinonitrile

di-n-propylamine

→

2-chloro-6-methylisonicotinonitrile

2-(dipropylamino)-6-methylisonicotinonitrile

반응 조건

후처리

1. 1
   기타Excess di-n-propylamine was removed under reduced pressure
2. 2
   기타the residue was partitioned between dichloromethane and aq. sodium bicarbonate
3. 3
   건조After drying over sodium sulfate and concentration
4. 4
   기타the residue was chromatographed on silica gel

실험 절차

To 2-chloro-6-methylisonicotinonitrile (0.230 g, 1.51 mmol) was added di-n-propylamine (5 mL). The mixture was heated at 80° C. in a sealed, thick-walled glass vessel for 12 h and then at room temperature for 17 h. Excess di-n-propylamine was removed under reduced pressure and the residue was partitioned between dichloromethane and aq. sodium bicarbonate. After drying over sodium sulfate and concentration, the residue was chromatographed on silica gel using ethyl acetate-hexane (10/90) to give 0.14 g of 2-chloro-6-methylisonicotinonitrile and 0.059 g of 2-(dipropylamino)-6-methylisonicotinonitrile. Using the above conditions, 2-chloro-6-methylisonicotinonitrile (0.14 g) was converted to an additional 0.043 g of 2-(dipropylamino)-6-methylisonicotinonitrile.

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