HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 59737515, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 771980 | HCID 771980 | — |
| Reactant | HCID 59737572 | HCID 59737572 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59737515 | HCID 59737515 | 47.6% |
Reaction Steps
To a solution of 243 (0.98 g, 1.81 mmol) in THF (10 mL) at 0° C., was added compound 246 (0.61 g, 2.17 mmol), triphenylphosphine (0.76 g, 2.89 mmol) and diethyl azodicarboxylate (DEAD) (0.51 g, 2.90 mmol), the ice bath was removed and the reaction mixture was allowed to stir at room temperature for 18 h. The reaction mixture was partitioned between EtOAc and H2O, organic phase was collected, washed successively with saturated NH4Cl and brine, dried over MgSO4, filtered and concentrated to give a light brown oil which was purified by flash chromatography (eluent: 50% AcOEt in hexanes to 100% AcOEt) to give intermediate 247 (0.65 g, 47% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598168B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-b6c480300144445099fba8523b47f449 |
| Source note | uspto-grants-2013_12 |