[NH2:1][C:2]([CH3:10])([CH2:8][CH3:9])[CH2:3][C:4](=O)[CH2:5][CH3:6].[C:11]1(=O)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.[Br-].[NH4+:19].N.C(=O)([O-])[O-].[K+].[K+]>CO>[CH2:5]([C:4]1[CH2:3][C:2]([CH2:8][CH3:9])([CH3:10])[NH:1][C:11]2([CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:19]=1)[CH3:6]14.3 g of the 5-amino-5-methyl-3-heptanone thus obtained were dissolved in 100 ml of methanol, and 10.0 g of cyclohexanone and 10.0 g of ammonium bromide were added to the resulting solution. Dry ammonia was then introduced into the solution at room temperature for 6 hours. The solution was then allowed to stand overnight, after which 10.0 g of potassium carbonate were added and the methanol was removed by evaporation under reduced pressure. The residue was extracted with benzene, and the benzene extract was washed with water and then dried over potassium carbonate. After removing the benzene, the residue was distilled under reduced pressure, giving 14.0 of 2,4-diethyl-4-methyl-1,5-diazaspiro[5.5]undec-1-ene (bp 93° - 94° C/1.5 mmHg).
Wird geladen…
