HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → benzyl N-[(2S)-4-[(2S)-2-[[(2S,3S)-3-methyl-1-(2-methylpropylamino)-1-oxopentan-2-yl]carbamoyl]pyrrolidin-1-yl]-3-oxo-1-phenylbutan-2-yl]carbamate;molecular nitrogen
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyloxycarbon-yl-l-phenylalanylbromomethane | HCID 11383290 | — |
| Reactant | N2 L-prolyl-N1-isobutyl-L-isoleucinamide | HCID 86746218 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | benzyl N-[(2S)-4-[(2S)-2-[[(2S,3S)-3-methyl-1-(2-methylpropylamino)-1-oxopentan-2-yl]carbamoyl]pyrrolidin-1-yl]-3-oxo-1-phenylbutan-2-yl]carbamate;molecular nitrogen | HCID 86746217 | — |
Reaction Steps
A solution of 8.86 g of [N-(benzyloxycarbonyl)-L-phenylalanyl]methyl bromide 6.71 g of N2 -L-prolyl-N1 -isobutyl-L-isoleucinamide and 2.60 g of triethylamine in 400 ml of dichloromethane was stirred at room temperature overnight. The solvent was removed by evaporation and the crude product was chromatographed on silica gel using ethyl acetate for the elution. The resulting product was triturated with a mixture of petroleum ether (b.p. 40°-60° C.) and ethyl acetate to give 8.70 g of N2 -[N-[[N-(benzyloxycarbonyl)-L-phenylalanyl]methyl]-L-prolyl]-N1 -isobutyl-L-isoleucinamide as an off-white solid of m.p. 80°-81° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05620987 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-02e530afd01f466db8e69538d386e852 |
| Source note | uspto-grants-1997_04 |