HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Thiomorpholine → 4-[[(4-Thiomorpholinyl)methylene]amino]-3-pyridinol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Thiomorpholine | HCID 67164 | — |
| Edukt | 4-[[(Dimethylamino)methylene]amino]-3-pyridinol | HCID 15380929 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 4-[[(4-Thiomorpholinyl)methylene]amino]-3-pyridinol | HCID 15380938 | — |
Reaktionsschritte
A mixture prepared from 4-[[(dimethylamino)methylene]amino]-3-pyridinol (5.14 g), thiomorpholine (10.5 ml, distilled from CaH2) and dry toluene (120 ml) was refluxed overnight. The reaction mixture was concentrated, triturated with diethyl ether, adhered to silica (methanol), flash chromatographed (10% methanol/ethyl acetate), and triturated with diethyl ether to yield 6.06 g of product. A 3.5 g sample was recrystallized from methanol, and dried under high vacuum and refluxing isopropanol to yield 2.13 g of crystals, m.p. 197°-198.5° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05869480 |
| Quelldatensatz | uspto-grants-1999_02 |
| ORD ID | ord-291c42efa7ff47deaf37615e4e62ac96 |
| Quellennotiz | uspto-grants-1999_02 |