HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloromethane methanol → HCID 178516473, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloromethane methanol | HCID 21226129 | — |
| Edukt | 5-[([4H,5H,6H-cyclopenta[b]thiophen-2-yl]amino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 86708080 | — |
| Lösungsmittel | Diphenyl Ether | HCID 7583 | — |
| Produkt | HCID 178516473 | HCID 178516473 | 80% |
Reaktionsschritte
A solution of 5-[([4H,5H,6H-cyclopenta[b]thiophen-2-yl]amino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione (540 mg, 1.84 mmol, 1.00 equiv) in phenoxybenzene (5 mL) was heated at 220° C. for 30 min under nitrogen. After cooling to room temperature, the residue was applied onto a silica gel column with dichloromethane/methanol (10:1) to give the desired 7-thia-9-azatricyclo[6.4.0.0^[2,6]]dodeca-1(8),2(6),9,11-tetraen-12-ol (0.28 g, 80%) as a brown solid. MS (ES): m/z 192 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09067948B2 |
| Quelldatensatz | uspto-grants-2015_06 |
| ORD ID | ord-5d3ae8ed2b5b45dc9dcdb05b460367a1 |
| Quellennotiz | uspto-grants-2015_06 |