HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Aluminium lithium hydride → [1-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-pyrrolidin-3-yl]-methanol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Edukt | 1-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-5-oxo-pyrrolidine-3-carboxylic acid methyl ester | HCID 66727299 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | [1-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-pyrrolidin-3-yl]-methanol | HCID 62372448 | — |
Reaktionsschritte
To a solution containing 130 mg (0.45 mmol) of 1-(2,3-dihydro-benzo[1,4]dioxin-2-ylmethyl)-5-oxo-pyrrolidine-3-carboxylic acid methyl ester in dry tetrahydrofuran (4 mL) was added 68 mg (1.79 mmol) of LiAlH4. The reaction mixture was stirred at room temperature for 2½ h, and subsequently refluxed for 2 h. After the reaction mixture was cooled to room temperature, it was quenched with water and 1 M NaOH. The solution was filtered through celite and the filtrate was evaporated to dryness. Purification by column chromatography (silica gel, triethylamine/ethyl acetate, 1:99) afforded the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08492549B2 |
| Quelldatensatz | uspto-grants-2013_07 |
| ORD ID | ord-3228913956fb45508929fbe086c84a0c |
| Quellennotiz | uspto-grants-2013_07 |