HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trifluoromethanesulfonic acid → N-[2-(1,3-Dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-O-2-propenyl-L-serine, methyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Edukt | Allyl 2,2,2-Trichloroacetimidate | HCID 316905 | — |
| Edukt | N-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-L-serine, methyl ester | HCID 67799768 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Dichloromethane cyclohexane | HCID 21916607 | — |
| Produkt | N-[2-(1,3-Dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-O-2-propenyl-L-serine, methyl ester | HCID 70044917 | — |
Reaktionsschritte
Dissolve N-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-L-serine, methyl ester (25 g, 63 mmol) in methylene chloride/cyclohexane (1:1, 600 mL). Add allyl trichloroacetimidate (26 g, 128 mmol) and trifluoromethanesulfonic acid (5 mL), 56.6 mmol). Stir at room temperature under a nitrogen atmosphere for 5 hours and dilute with methylene chloride. Wash with saturated aqueous sodium hydrogen carbonate, water, dry (MgSO4) and evaporate the solvent in vacuo. Purify by silica gel chromatography (gradient 20% ethyl acetate/hexane to 35% ethyl acetate/hexane) to give the title compound; mp 95°-97° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05624921 |
| Quelldatensatz | uspto-grants-1997_04 |
| ORD ID | ord-53daaa13c7c44265b8e1c126d7b9a493 |
| Quellennotiz | uspto-grants-1997_04 |