HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (S)-Methyl 1-((S)-2-(((benzyloxy)carbonyl)amino)-3-methylbutanoyl)pyrrolidine-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Reactant | N-Carbobenzoxy-L-valine | HCID 726987 | — |
| Reactant | methyl L-prolinate hydrochloride | HCID 2733200 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (S)-Methyl 1-((S)-2-(((benzyloxy)carbonyl)amino)-3-methylbutanoyl)pyrrolidine-2-carboxylate | HCID 14032133 | — |
Reaction Steps
To a solution of N-Cbz-valine (2.5 g, 10 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (1.6 g, 11 mmol) and triethylamine (2.0 g, 20 mmol) in DMF (10 mL) is added dropwise a solution of proline methyl ester hydrochloride (1.8 g, 11 mmol) in DMF (5 mL). The solution is stirred at room temperature and the reaction monitored by TLC until the disappearance of N-Cbz-valine. The reaction solution is then diluted with dichloromethane (30 mL) and the organic layer is extracted with 0.1 N HCl (20 mL), water (20 mL), then dried over Na2SO4. The solvent is removed in vacuo to afford the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09011918B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-974f3656bbd14ffda6cf5283d4695c19 |
| Source note | uspto-grants-2015_04 |