HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → Benzyl 1,4-diazepane-1-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Benzyl chloroformate | HCID 10387 | — |
| Edukt | Hexahydro-1,4-diazepine | HCID 68163 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | Benzyl 1,4-diazepane-1-carboxylate | HCID 4384955 | 65,5% |
Reaktionsschritte
To 230 ml of dimethylformamide were added 25 g of homopiperazine and 5.4 g of sodium bicarbonate and then 25 ml of water followed by dropwise addition of 10 g of benzyloxycarbonyl chloride with stirring under ice cooling, and the mixture was stirred at a room temperature overnight. After evaporating off dimethylformamide under a reduced pressure, the reaction mixture was extracted three times with 100 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (9:1), to obtain 9 g of the title compound as a light yellow liquor liquid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05245034 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-9210acb815974a8380d54b730e8abe69 |
| Quellennotiz | uspto-grants-1993_09 |