HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → HCID 178503420, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Zinc | HCID 23994 | — |
| Edukt | 5-(2-(Methylthio)-4-pyrimidinyl)-2-thiophenesulfonyl chloride | HCID 2736995 | — |
| Lösungsmittel | Oxolane--water (1/1) | HCID 21881883 | — |
| Produkt | HCID 178503420 | HCID 178503420 | 236,8% |
Reaktionsschritte
Zinc dust (106.5 mg, 1.63 mmol) in THF/H2O (2:1, 7.5 mL) was sonicated 15 minutes and 5-(2-Methylsulfanyl-pyrimidin-4-yl)-thiophene-2-sulfonyl chloride (500 mg, 1.63 mmol) was added all at once as a solid. After 22 hours, the mixture was concentrated to ¼ volume and a precipitate formed. Water was added and the suspension was sonicated for 1 minute. The solids were collected by filtration, washed with water and dried in vacuo to afford bis-5-(2-Methylsulfanyl-pyrimidin-4-yl)-thiophene-2-sulfonyl Zinc as a light yellow solid (1.3 g, >100%). This material was used in the next step. 1H NMR (500 MHz, DMSO-d6) δ 2.52 (s, 3H), 7.15 (d, J=3.5 Hz, 1H), 7.59 (d, J=5.5 Hz, 1H), 7.88 (d, J=3.5 Hz, 1H), 8.54 (d, J=5.5 Hz, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07977481B2 |
| Quelldatensatz | uspto-grants-2011_07 |
| ORD ID | ord-f9a4331eddaf4ce7a1513e59357c3d25 |
| Quellennotiz | uspto-grants-2011_07 |