HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 22975787, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | tert-Butyl (9-benzyl-3,9-diazaspiro[5.5]undecan-3-yl)acetate | HCID 22975805 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 22975787 | HCID 22975787 | — |
Reaction Steps
To a solution of 9.3 g (25.9 mmol) of the compound from Step E in 400 ml dry ethanol were added 1.5 ml acetic acid and 0.7 g Pd(II) hydroxide. The mixture was filled into an autoclave and hydrogenated at 50 atm and 50° C. for 18 h. The solvent was removed under reduced pressure, and the residue was stirred with saturated aqueous sodium bicarbonate solution. It was extracted five times with 100 ml tert.-butylmethylether followed by three extractions with 100 ml dichloromethane. The extracts were dried over sodium sulfate and concentrated in vacuo, separately. The first extract contained a mixture of compounds, whereas the pure title intermediate was obtaind from the following.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06291469B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-6901965738e9492ca39fd60430c4e052 |
| Source note | uspto-grants-2001_09 |