HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → (R)-3-((R)-2-Cyclopentyl-2-hydroxy-2-phenylacetoxy)pyrrolidine-1-carboxylic acid t-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | tert-Butyl (3S)-3-hydroxypyrrolidine-1-carboxylate | HCID 854055 | — |
| Reactant | alpha-Cyclopentylmandelic acid, (+)- | HCID 948620 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (R)-3-((R)-2-Cyclopentyl-2-hydroxy-2-phenylacetoxy)pyrrolidine-1-carboxylic acid t-butyl ester | HCID 57613514 | 282.8% |
Reaction Steps
(R)-Cyclopentylhydroxyphenylacetic acid (20 g, 90.8 mmol), (S)-3-hydroxypyrrolidine-1-carboxylic acid t-butyl ester (18 g, 96.2 mmol) and triphenylphosphine (24 g, 91.5 mmol) were dissolved in THF (100 mL). Diisopropyl azodicarboxylate (19.7 mL, 99.9 mmol) was added slowly at room temperature. The mixture was stirred overnight at room temperature. The solvent was removed by rotary evaporation. EtOAc was then added and the solution was washed with a saturated NaHCO3 solution, then saturated aqueous NaCl. The organic layer was dried over Na2SO4 then concentrated to yield approximately 100 g of crude title compound, which was used immediately without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08017617B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-345d450df8f94a8bbafccc21e3ef0a56 |
| Source note | uspto-grants-2011_09 |