HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid [4-(Pyrimidin-2-ylsulfamoyl)-phenyl]-amide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | 4-Piperazinopyrido[3',2';4,5]thieno[3,2-d]pyrimidine | HCID 67390286 | — |
| Edukt | N-Pyrimidin-2-yl-4-thioformylamino-benzenesulfonamide chloride | HCID 86601004 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid [4-(Pyrimidin-2-ylsulfamoyl)-phenyl]-amide | HCID 59020502 | — |
Reaktionsschritte
To a solution of 4-piperazinopyrido[3′,2′;4,5]thieno[3,2-d]pyrimidine (200 mg, 0.74 mmol) and pyridine (0.5 mL, 7.9 mmol) in dichloromethane (20 mL) was added a solution of product 1d in dichloromethane (20 mL) and this was stirred overnight. Methanol was added to quench excess thiophosgene, and the residue after removal of solvent was purified by silica gel column chromatography eluting with 5% methanol/dichloromethane and further recrystallized from dichloromethane/hexane to give 60 mg (15%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08552018B2 |
| Quelldatensatz | uspto-grants-2013_10 |
| ORD ID | ord-2652a11ed59e4b07ae29fe0095d0b451 |
| Quellennotiz | uspto-grants-2013_10 |