HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → 5,6-Dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | (Dimethyl sulfide)trihydroboron | HCID 12423031 | — |
| Edukt | 5,6-dihydro-4H-[1,2,4]-triazolo-[4,3-a][1,5]benzodiazepin-5-one | HCID 21837128 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 5,6-Dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine | HCID 21837004 | — |
Reaktionsschritte
A mixture of 7.0 g of 5,6-dihydro-4H-[1,2,4]-triazolo-[4,3-a][1,5]benzodiazepin-5-one in 25 ml of tetrahydrofuran is added 9 ml of 10M borane-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 6 hours, cooled to room temperature and 25 ml of methanol added dropwise. The volatiles are removed under vacuum and to the residue is added 100 ml of 2N sodium hydroxide. The mixture is refluxed for 5 hours, chilled and extracted with dichloromethane. The extract is washed with 2N citric acid, water and dried (Na2SO4). The solvent is removed under vacuum to give a solid. The solid is purified by chromatography on silica gel to give the desired product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05733905 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-44ee38b3384d451c8b68f82532c2510d |
| Quellennotiz | uspto-grants-1998_03 |