HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodoethane → (4R)-1-Boc-4-ethoxy-L-proline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | (2S,4R)-4-hydroxy-1-[(2-methylpropan-2-yl)oxycarbonyl]pyrrolidine-2-carboxylic acid | HCID 88804 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (4R)-1-Boc-4-ethoxy-L-proline | HCID 15222301 | 82.8% |
Reaction Steps
1.72 g of 60% sodium hydride in oil are added, under a nitrogen atmosphere, to a solution of 5 g of (2S,4R)-1-(tert-butoxycarbonyl)-4-hydroxy-2-pyrrolidinecarboxylic acid in 100 ml of THF, and the mixture is stirred for 45 minutes at RT. 3.27 g of ethyl iodide are then added, the mixture is refluxed for 3 hours and stirred for 18 hours while allowing the temperature to return to RT. The reaction mixture is concentrated under vacuum, the residue is taken up in 5% KHSO4 solution and extracted with EtOAc, the organic phase is dried over Na2SO4 and the solvent is evaporated off under vacuum. 4.5 g of the expected product are obtained in the form of an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07297692B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-47719d4aa89f4acaab78fcec0dd42494 |
| Source note | uspto-grants-2007_11 |