반응 #465568

반응 방정식

3,3,6,6,-tetramethyl-1,2-cyclohexanedione

1,2-cyclohexanediamine

water

→

title compound

1,2,3,4,6,7,8,9-octahydro-6,6,9,9-tetramethylphenazin-1-one

용매

acetic acid

반응 조건

후처리

1. 1
   온도The obtained solution was heated
2. 2
   온도under reflux for 6 hours
3. 3
   온도cooled
4. 4
   추출followed by the extraction with ethyl acetate
5. 5
   세척The organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate
6. 6
   건조a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
7. 7
   농축concentrated in a vacuum
8. 8
   기타The obtained residue was purified by silica gel chromatography (developer: 5% ethyl acetate/hexane)

실험 절차

20.0 g of 3,3,6,6,-tetramethyl-1,2-cyclohexanedione and 20 ml of 1,2-cyclohexanediamine were dissolved in 20 ml of acetic acid. The obtained solution was heated under reflux for 6 hours, cooled by allowing to stand, and poured into water, followed by the extraction with ethyl acetate. The organic phase was washed with a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate, and concentrated in a vacuum. The obtained residue was purified by silica gel chromatography (developer: 5% ethyl acetate/hexane) to give 16.0 g of the title compound as a colorless oil.

출처