HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic acid, 2-chloro-, phenylmethyl ester → HCID 67506082, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic acid, 2-chloro-, phenylmethyl ester | HCID 8786 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | methyl L-prolinate hydrochloride | HCID 2733200 | — |
| Catalyst | Tetrabutylammonium Iodide | HCID 67553 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67506082 | HCID 67506082 | — |
Reaction Steps
To a solution of chloroacetic benzyl ester (1.8 g, 9.75 mmol) in DCM (50 mL) is added (S)-pyrrolidine-2-carboxylic acid methyl ester hydrochloride (1.51 g, 11.70 mmol), diisopropylethylamine (4.09 mL, 23.40 mmol) and tetrabutylammonium iodide (3.60 g, 9.75 mmol) and the resulting mixture is stirred at room temperature overnight. The solvent is removed under reduced pressure and the residue purified by column chromatography using a gradient of 2-45% EtOAc/heptane to give (S)-1-benzyloxycarbonylmethyl-pyrrolidine-2-carboxylic acid methyl ester; 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.81-2.05 (m, 3H), 2.13-2.24 (m, 1H), 2.78-2.84 (m, 1H), 3.15-3.20 (m, 1H), 3.57-3.69 (m, 3H), 3.70 (s, 3H), 5.15 (s, 2H), 7.36 (m, 5H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08993631B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-793ef0fd9cdf465483cf459c2d8a7937 |
| Source note | uspto-grants-2015_03 |