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 | — |
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 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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04097587 |
| Source dataset | uspto-grants-1978_06 |
| ORD ID | ord-cb6c15dbdd7a4a17b5dcec5fb6bee2e8 |
| Source note | uspto-grants-1978_06 |