HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 53791264, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl L-valinate hydrochloride | HCID 87181 | — |
| Reactant | N-Carbobenzoxy-L-valine | HCID 726987 | — |
| Reactant | Methanesulfonic acid, 1H-benzotriazol-1-yl ester | HCID 11745953 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 53791264 | HCID 53791264 | 90.3% |
Reaction Steps
N-Benzyloxycarbonyl-L-valine (1.25 g) and L-valine ethyl ester hydrochloride (1.08 g) are dissolved in dichloromethane (15 ml) and thereto are added triethylamine (1.54 ml) and further 1-methanesulfonyloxy-1,2,3-benzotriazole (1.07 g) under ice-cooling. After allowing to stand at room temperature for 72 hours, to the reaction mixture are added water and ethyl acetate. The ethyl acetate layer is separated, washed with water, dried and then the solvent is distilled off to give N-(N-benzyloxycarbonyl-L-valyl)-L-valine ethyl ester (1.70 g). The product is washed with petroleum ether to give powdery product (1.50 g), melting point: 93°-93.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04242507 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-17cc5afabcf343908833d02695e8372c |
| Source note | uspto-grants-1980_12 |