반응 #65142

반응 방정식

5-bromo-1,2-dihydro-2,2-dimethyl-6-(2-imidazolin-2-ylamino)-3-(4H)-quinoxalinone

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title compound

5-bromo-2,2-dimethyl-6-(2-imidazolin-2-ylamino)-1,2,3,4-tetrahydroquinoxaline

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도is heated
2. 2
   온도maintained at a temperature of 50°-80° C. until the starting material
3. 3
   기타is consumed
4. 4
   workup.ADDITION2-3 drops of H2O is added
5. 5
   여과the mixture is filtered
6. 6
   농축The solution is concentrated in vacuo
7. 7
   기타to yield a residue which
8. 8
   기타is chromatographed on silica gel with CHCl3
9. 9
   세척CH3OH saturated with NH3 (g) elution

실험 절차

A suspension of 5-bromo-1,2-dihydro-2,2-dimethyl-6-(2-imidazolin-2-ylamino)-3-(4H)-quinoxalinone (150 mg, 0.45 mmol) and LiALH4 (17 mg, 0.45 mmol) in tetrahydrofuran (3 ml) is heated and maintained at a temperature of 50°-80° C. until the starting material is consumed. The mixture is cooled to 0° C., 2-3 drops of H2O is added and the mixture is filtered. The solution is concentrated in vacuo to yield a residue which is chromatographed on silica gel with CHCl3 : CH3OH saturated with NH3 (g) elution to produce the title compound.

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