HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → HCID 178435041, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | N-benzoyl-N'-(3-cyano-4,5-dimethyl-2-thienyl)thiourea | HCID 899430 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178435041 | HCID 178435041 | 87,1% |
Reaktionsschritte
A solution of N-(3-cyano-4,5-dimethylthiophen-2-ylcarbamothioyl)benzamide (example 1a) (1.90 g, 6.03 mmol) and NaOH (2 N, 8.3 mL) in EtOH (25 mL) was stirred at 100° C. under nitrogen for half an hour. After cooling to room temperature, the clear reaction solution was filtered and the filtrate was carefully neutralized with 10% AcOH with vigorous stirring at 0° C. The resultant precipitate was collected by filtration, washed with warm water and then 20% EtOH in water to give the final product 4-amino-5,6-dimethylthieno[2,3-d]pyrimidine-2(1H)-thione (1.11 g, 87%) as an off-white solid. M.p.: >260° C. 1H NMR (400 MHz, DMSO-d6) δ2.25 (s, 3H), 2.26 (s, 3H). MS 212 (MH+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08541421B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-580783d52bf64d1c8c5dd8ecf4dc013e |
| Quellennotiz | uspto-grants-2013_09 |