HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium bifluoride → HCID 118380314, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium bifluoride | HCID 14935 | — |
| Edukt | Cloperastine Hydrochloride | HCID 161104 | — |
| Edukt | HCID 140689321 | HCID 140689321 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | HCID 22708839 | HCID 22708839 | — |
| Produkt | HCID 118380314 | HCID 118380314 | 99,5% |
Reaktionsschritte
Prepared according to Seki et al. Synlett 1995, 609-611. To a solution of tert-butyl 2-(((Z)-(1-(2-((tert-butoxycarbonyl)amino)thiazol-4-yl)-2-(((2R,3S)-2-(((2-((tert-butyldimethylsilyl)oxy)ethyl)amino)methyl)-4-oxoazetidin-3-yl)amino)-2-oxoethylidene)amino)oxy)-2-methylpropanoate (111 mg, 0.162 mmol) in DMF:NMP (2.7:1, 1.62 mL) was added ammonium fluoride hydrofluoride (37.0 mg, 0.648 mmol). After stirring for 65 h, the solution was diluted with water and extracted with EtOAc. The organic layer was dried over sodium sulfate and concentrated in vacuo to afford crude title compound (92 mg, 99%). The crude material was used directly in step 3. LCMS: R=0.76 min, m/z 571.3 (M+1) Method 2m_acidic.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09174978B2 |
| Quelldatensatz | uspto-grants-2015_11 |
| ORD ID | ord-7dc75cf636b5476cab09d566abb21a73 |
| Quellennotiz | uspto-grants-2015_11 |