HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,4-Dioxane → HCID 57377355, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,4-Dioxane | HCID 31275 | — |
| Edukt | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Edukt | Methyl 4-(1-(5-chloro-2-(3-((3-fluorophenoxy)methyl)pyrrolidin-1-yl)nicotinamido)cyclopropyl)benzoate | HCID 67958339 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 57377355 | HCID 57377355 | 51% |
Reaktionsschritte
To a solution of methyl 4-(1-(5-chloro-2-(3-((3-fluorophenoxy)methyl)pyrrolidin-1-yl)nicotinamido)cyclopropyl)benzoate (D200) (37 mg, 0.070 mmol) in a mixture 1,4-dioxane and water (3:1) (2 ml) lithium hydroxide monohydrate (10 mg, 0.238 mmol) was added and the mixture was stirred 20 min (4 cycles of 5 min each) under microwaves irradiation. After solvent evaporation the residue was diluted with water (5 ml) and 1M HCl (5 ml) and extracted with ethylacetate (3×10 ml). Collected organics after solvent evaporation afforded a residue that was purified by ISOLUTE Spe-Si (1 g) eluting with a mixture dichloromethane/methanol 98:2. Collected fractions after solvent evaporation afforded the title compound (E76) (18.2 mg)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08828987B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-75ba6ba62431407f8959d271c8005641 |
| Quellennotiz | uspto-grants-2014_09 |