HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86756663, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | HCID 15545387 | HCID 15545387 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86756663 | HCID 86756663 | 76% |
Reaction Steps
To a solution of (2R,3aS)-2-hydroxy-5-[4-[(2-phenylbenzoyl)amino]benzoyl]-1,2,3,3a,4,5-hexahydro-pyrrolo[1,2-a]quinoxaline (0.8 g) prepared in Example 3, acetic acid (0.15 g) and triphenyl phosphine (0.64 g) in anhydrous tetrahydrofuran (5 ml), there was gradually dropwise added a solution of diisopropyl azodicarboxylate (0.49 g) in anhydrous tetrahydrofuran (2 ml) under ice-cooling. After stirring the reaction solution at room temperature for 2 hours, it was concentrated. The resulting residue was subjected to silica gel column chromatography and then eluted with hexane/ethyl acetate (1/1) to give 0.66 g (yield 76.0%) of the title compound as amorphous powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06225306B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-f50b9e06289744599a4464c3b11b2af3 |
| Source note | uspto-grants-2001_05 |