HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 1-Ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Boron tribromide dichloromethane | HCID 22277759 | — |
| Edukt | 1-Ethyl-7-methoxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68674307 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-Ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68673385 | 98% |
Reaktionsschritte
A 1.0 M boron tribromide/dichloromethane solution (1.22 ml) was added to a dichloromethane solution (3 ml) of 1-ethyl-7-methoxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (169 mg, 1.0 mmol) at 0° C., and stirred at room temperature overnight. Water and methanol were added to the reaction mixture and extraction with the mixture solvent (dichloromethane:methanol=10:1) was performed. The organic layer was dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure to thereby obtain 156.4 mg (yield: 98%) of 1-ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione as a white powder.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08664217B2 |
| Quelldatensatz | uspto-grants-2014_03 |
| ORD ID | ord-281abd54973f4ae0a01c7037fd84cdff |
| Quellennotiz | uspto-grants-2014_03 |