HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chloroform → 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chloroform | HCID 6212 | — |
| Edukt | Hexane | HCID 8058 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 2-Amino-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3h)-one | HCID 290197 | — |
| Lösungsmittel | Acetic Anhydride | HCID 7918 | — |
| Produkt | 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine | HCID 12910200 | 44% |
Reaktionsschritte
To a 50 mL flask was added 10 (221 mg, 1 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added mL of CHCl3 and 300 mg of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane: acetyl acetate=20:1 as eluent afford 105 mg (44%) of 11 as a yellow solid:
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09045489B2 |
| Quelldatensatz | uspto-grants-2015_06 |
| ORD ID | ord-5b6ecdc450014a279d6ce94d592fc4f8 |
| Quellennotiz | uspto-grants-2015_06 |