HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 66616133, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Triphenylphosphine Oxide | HCID 13097 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 66616121 | HCID 66616121 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66616133 | HCID 66616133 | — |
Reaction Steps
To a mixture of (S)—N-(1-(4-(3,3-dimethyl-2-oxoindolin-1-yl)piperidin-1-yl)-1-oxo-4-phenylbutan-2-yl)-2-nitrobenzenesulfonamide (1.26 g, 2.13 mmol, EXAMPLE 73, Step 1), methanol (519 microL, 12.8 mmol), triphenylphosphine (1.12 g, 4.27 mmol) in tetrahydrofuran (10 mL) was added diethyl azodicarboxylate (2.2 mol/L toluene solution, 3.88 mL, 8.53 mmol) at room temperature. After 3 h, the mixture was concentrated and the residue was purified by silica gel column chromatography (hexane/ethyl acetate, gradient) to give a mixture of the title compound and triphenylphosphineoxide (3.30 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697877B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-417b8931f8504c4e9a110ae6dd51ddd4 |
| Source note | uspto-grants-2014_04 |