HuagongsheHuagongshe Chemistry Print Report · For research reference only
Di-tert-butyl dicarbonate → HCID 131735925, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | HCID 89649170 | HCID 89649170 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131735925 | HCID 131735925 | 62.4% |
Reaction Steps
To a solution of (5R)-2-(4-bromo-3-methyl-2-pyridyl)-7-methyl-1,7-diazaspiro[4.4]nonan-6-one (which may be prepared as described in Description 10) (554.4 mg, 0.8500 mmol) in DCM (2 mL) was added and tert-butoxycarbonyl tert-butyl carbonate (373.2 mg, 1.71 mmol) the reaction was then stirred at room temperature for 3 days. The reaction was concentrated in vacuo and the residue was purified by silica gel chromatography, eluting with EtOAc in isohexane from 0% to 100%. A slower running material was isolated tert-butyl (2R,5R)-2-(4-bromo-3-methyl-2-pyridyl)-7-methyl-6-oxo-1,7-diazaspiro[4.4]nonane-1-carboxylate (D98) (225.1 mg, 0.5305 mmol, 62% yield) as a colourless oil; M/Z: 423.8, 425.9 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09376436B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-5c05051bbe4b42a29a33f14e0f6a491f |
| Source note | uspto-grants-2016_06 |