HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,8-Diazabicyclo(5.4.0)undec-7-ene → 5-tert-Butyl-3-(2-chloro-benzyl)-7-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Edukt | 1,3-Propanesultam | HCID 642157 | — |
| Edukt | 5-tert-butyl-7-chloro-3-(2-chlorobenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine | HCID 86683284 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 5-tert-Butyl-3-(2-chloro-benzyl)-7-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine | HCID 86683290 | 16% |
Reaktionsschritte
A mixture of 5-tert-butyl-7-chloro-3-(2-chlorobenzyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine (15.9 mg, 47.2 μmol), 1,1-dioxo-isothiazolidine (11.4 mg, 94.4 μmol) and DBU (14.2 μL, 94.4 μmol) in DMF (250 μL) was stirred at the room temperature overnight. The reaction mixture was directly purified by preparative HPLC (column: Gemini Sum C18 110A 75×30 mm. mobile phase: water (0.05% Et3N): acetonitrile 75:25% to 5:95%. WL: 230 nm Flow: 30 mL/min.) to afford the title compound as white solid (3.10 mg, 16%). MS (m/e): 387.3 (MH+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08741906B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-80588c1206c5471db8ded5e80daec0fa |
| Quellennotiz | uspto-grants-2014_06 |