HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tributylphosphine → {4-[3-Bromo-5-(3-morpholin-4-yl-propoxy)-phenylsulfanyl]-2-chloro-phenoxy}-acetic Acid Ethyl Ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tributylphosphine | HCID 13831 | — |
| Edukt | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Edukt | 3-Morpholino-1-propanol | HCID 199576 | — |
| Edukt | [4-(3-Bromo-5-hydroxy-phenylsulfanyl)-2-chloro-phenoxy]-acetic Acid Ethyl Acetate | HCID 67024266 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | {4-[3-Bromo-5-(3-morpholin-4-yl-propoxy)-phenylsulfanyl]-2-chloro-phenoxy}-acetic Acid Ethyl Ester | HCID 57791920 | — |
Reaktionsschritte
[4-(3-Bromo-5-hydroxy-phenylsulfanyl)-2-chloro-phenoxy]-acetic acid ethyl acetate (1.7 g; 4.07 mmol), N-(3-hydroxypropyl)morpholine (0.59 g; 4.07 mmol) and tributylphosphine (1.8 g; 7.33 mmol) were dissolved in THF (100 mL) in a dried reaction flask under an atmosphere of nitrogen. 1,1′-(Azodicarbonyl)dipiperidine (1.85 g; 7.33 mmol) dissolved in THF (50 mL) was added to the reaction mixture, which was stirred at room temperature for 16 h. The reaction mixture was evaporated to dryness and purified by flash chromatography (ethyl acetate:heptane). Yield: 1.1 g. HPLC-MS: m/z: 544.0 (M+); Rt: 1.78 min.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07943669B2 |
| Quelldatensatz | uspto-grants-2011_05 |
| ORD ID | ord-ae040c11c28b47dcb2c53d3addc235f1 |
| Quellennotiz | uspto-grants-2011_05 |