HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Chloroaniline → 2-chloro-N-(3-chlorophenyl)-9H-purin-6-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Chloroaniline | HCID 7932 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2,6-Dichloropurine | HCID 5324412 | — |
| Edukt | Chloroform methanol | HCID 21584188 | — |
| Lösungsmittel | 1-Butanol | HCID 263 | — |
| Produkt | 2-chloro-N-(3-chlorophenyl)-9H-purin-6-amine | HCID 21988232 | — |
Reaktionsschritte
2,6-Dichloropurine (3.78 g; 0.02 mol) was reacted with 3-chloroaniline (3.83 g; 0.03 mol) in n-butanol (40 ml) in the presence of triethylamine (7 ml; 0.05 mol) at 110° C. for 3 hours. After cooling to room temperature the reaction mixture was stirred at 0° C. for 2 hours. The yellow precipitate was filtered off, washed with cold n-butanol (2×10 ml), water (3×10 ml) and dried in the drying oven at 60° C. into constant weight. Yield: 3.69 g yellow crystalline powder (65.8%). The crude product was crystallized from isopropanol to give 2.85 g of pure substance. TLC (chloroform-methanol; 85:15): one single spot; free of starting material. HPLC purity: 98+%
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08222260B2 |
| Quelldatensatz | uspto-grants-2012_07 |
| ORD ID | ord-21a364d405924444819268b98b8a5a3c |
| Quellennotiz | uspto-grants-2012_07 |