HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 2,4-Diethyl-4-methyl-1,5-diazaspiro[5.5]undec-1-ene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Cyclohexanone | HCID 7967 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ammonium Bromide | HCID 25514 | — |
| Reactant | 5-Amino-5-methylheptan-3-one | HCID 21330457 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2,4-Diethyl-4-methyl-1,5-diazaspiro[5.5]undec-1-ene | HCID 21330454 | 63.1% |
Reaction Steps
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 a period of 6 hours. After allowing the solution to stand overnight, 10.0 g of potassium carbonate were added and the methanol was then removed by distillation under reduced pressure. The residue was extracted with benzene, washed with water and dried over potassium carbonate. The benzene was then removed and the residue was distilled under reduced pressure, giving 14.0 g of 2,4-diethyl-4-methyl-1,5-diazaspiro[5.5]-undec-1-ene (bp 93° - 94° C/1.5 mmHg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04075165 |
| Source dataset | uspto-grants-1978_02 |
| ORD ID | ord-87fe7d87698f4025b9c2de6357c6ed4c |
| Source note | uspto-grants-1978_02 |