HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
L-Aspartic Acid → 4-tert-Butyl hydrogen L-aspartate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | L-Aspartic Acid | HCID 5960 | — |
| Edukt | Fmoc-L-Asp(OtBu)-OH | HCID 2724635 | — |
| Lösungsmittel | Dichloromethane piperidine | HCID 67144590 | — |
| Produkt | 4-tert-Butyl hydrogen L-aspartate | HCID 7010570 | 110,1% |
Reaktionsschritte
Synthesis of Asp(OtBuj-OH. Fmoc-Asp(OtBu)-OH (500 mg, 1.2 mmole) was dissolved in a 9:1 mixture of dichloromethane-piperidine (5 mL) in a 25 mL round-bottomed flask. The reaction mixture was stirred overnight at room temperature. The next morning, TLC analysis indicated complete Fmoc deprotection. The reaction mixture was concentrated by rotoevaporation, coevaporated 2 times with toluene, and dried under vacuum to give a crude oil. This oil was purified by flash chromatography on silica gel (50 g) using a stepwise solvent gradient of 10%–50% methanol in dichloromethane to afford 250 mg (100%) of Asp(OtBu)-OH.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07148030B2 |
| Quelldatensatz | uspto-grants-2006_12 |
| ORD ID | ord-69e5d20e92f14e0aa90662250c458fb2 |
| Quellennotiz | uspto-grants-2006_12 |