HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → HCID 59255164, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Sodium borohydride | HCID 4311764 | — |
| Edukt | 2-(3-((E)-2-nitro-vinyl)-phenoxymethyl)-pyridine | HCID 59255249 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | HCID 59255164 | HCID 59255164 | 64,3% |
Reaktionsschritte
To an acetic acid (2.5 mL) and dimethyl sulfoxide (43 mL) solution of 2-(3-((E)-2-nitro-vinyl)-phenoxymethyl)-pyridine (2.56 g, 10 mmol) described in Manufacturing Example 60-1-2 was added sodium borohydride (605 mg, 16 mmol) at room temperature while cooling appropriately. This mixture was stirred for 1.5 hours at room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (heptane:ethyl acetate=10:1-4:1-1:1) to obtain the title compound (1.66 g, 64%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07691882B2 |
| Quelldatensatz | uspto-grants-2010_04 |
| ORD ID | ord-6617388db52243b89a5f9ffcdb0ed645 |
| Quellennotiz | uspto-grants-2010_04 |