HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 3,3-Dimethyl-1,5-dioxaspiro(5.5)undecan-9-one | HCID 587968 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamine | HCID 59970317 | — |
Reaction Steps
A solution of 20.0 g (0.1 mol) of 3,3-dimethyl-1,5-dioxaspiro[5.5]undecan-9-one in 250 ml of methanol which contained 38 g of ammonia was hydrogenated at 100° C. and a hydrogen pressure of 100 bar in the presence of 3 g of Raney nickel. The catalyst was filtered off and the solvent was stripped off in vacuo. The crude product was purified by means of a thin film evaporator (140° C./0.8 bar). This gave 16 g (80% of theory) of distillate which solidified upon standing.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05859009 |
| Source dataset | uspto-grants-1999_01 |
| ORD ID | ord-1f876b8756394ccf8b294e4ac8acb593 |
| Source note | uspto-grants-1999_01 |