HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 118390114, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | tert-Butyl 9-oxo-3-azaspiro[5.5]undecane-3-carboxylate | HCID 51072194 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 118390114 | HCID 118390114 | 46.2% |
Reaction Steps
To a solution of tert-butyl 9-oxo-3-azaspiro[5.5]undecane-3-carboxylate (2.15 g, 8.05 mmol) in EtOH (20 mL) was added 33% methanamine in EtOH (3.7 g, 40.3 mmol), and the mixture was stirred at r.t for 1.5 h. Then NaBH3CN (1.5 g, 24.2 mmol) was added to the mixture. After that the resulting mixture was stirred at r.t overnight and then concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=10/1) to give the product as brown oil (1.05 g, 46.2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403801B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-374889012e5a4580a53e174f214dfd50 |
| Source note | uspto-grants-2016_08 |