HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → 4-Benzyloxycarbonyl-1-(p-methoxybenzyl)-piperazin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| Edukt | Benzyl 3-oxopiperazine-1-carboxylate | HCID 736777 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 4-Benzyloxycarbonyl-1-(p-methoxybenzyl)-piperazin-2-one | HCID 69015787 | 54% |
Reaktionsschritte
Add to a solution of 4-benzyloxycarbonyl-piperazin-2-one (2 g, 8.6 mmol) in dry THF (10 mL/mmol) under nitrogen, sodium hydride (236 mg, 9.4 mmol, 60% dispersion in mineral oil) in one portion and stir at room temperature for 30 min. Add p-methoxybenzyl chloride (1.86 mL, 13 mmol) and stir at room temperature overnight. Concentrate, add ethyl acetate, wash with water, saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 1:1 hexanes:ethyl acetate) to give the title compound as an oil (1.6 g, 54%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07618978B2 |
| Quelldatensatz | uspto-grants-2009_11 |
| ORD ID | ord-474dca69fe854402817812a0ea1ea0c7 |
| Quellennotiz | uspto-grants-2009_11 |