HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 8-(3-Aminoazepan-1-yl)-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Azepan-3-amine | HCID 2756445 | — |
| Edukt | 8-Bromo-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione | HCID 22508575 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 8-(3-Aminoazepan-1-yl)-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione | HCID 22508638 | — |
Reaktionsschritte
8-Bromo-7-(2-bromobenzyl)-3-methyl-3,7-dihydropurine-2,6-dione (80A) (300 mg, 0,7 mmol) and azepan-3-ylamine (248 mg, 2,2 mmol), and triethylamine (0.5 ml, 3,6 mmol) were dissolved in 3 ml of DMSO and the mixture was subjected to microwaves (method F, 200° C., 300 W) for 30 minutes. To the reaction mixture was added 100 ml of water and 100 ml of dichloromethane, and the organic layer was separated and dried over sodium sulfate. The solvents were evaporated and the crude product was purified by preparative HPLC (method A1, Rt=7.17 min.). Evaporation of the solvent afforded the title compound as an brown oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07192952B2 |
| Quelldatensatz | uspto-grants-2007_03 |
| ORD ID | ord-f63a5f954fff49b69eb65b75e3ab1433 |
| Quellennotiz | uspto-grants-2007_03 |