HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → Tert-butyl 3-(dimethylamino)azetidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | 3-Oxo-azetidine-1-carboxylic acid tert-butyl ester | HCID 1519404 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Tert-butyl 3-(dimethylamino)azetidine-1-carboxylate | HCID 23145930 | 101% |
Reaction Steps
To a solution of 1-Boc-azetidin-3-one (3.45 g) in methanol (175 ml) were added a 2M solution of dimethylamine in tetrahydrofuran (21.9 ml), acetic acid (1.73 ml), 10% palladium on carbon (2.15 g), followed by stirring at room temperature under a hydrogen atmosphere for 14 hr. The catalyst was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and a saturated aqueous solution of sodium hydrogencarbonate. The combined organic layer was dried over anhydrous sodium sulfate, which was concentrated to provide the titled compound as a colorless oil (4.07 g, 101%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288538B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-609bffe2df6e4b6484bb6258abc75f4e |
| Source note | uspto-grants-2012_10 |