HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-(3-Methylphenylthio)methyl-5-fluoropyrimidin-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 5-Fluoropyrimidin-2-one | HCID 101498 | — |
| Edukt | Potassium Bromide | HCID 253877 | — |
| Edukt | 3-Methylphenyl chloromethyl sulfide | HCID 12840894 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-(3-Methylphenylthio)methyl-5-fluoropyrimidin-2-one | HCID 15650500 | — |
Reaktionsschritte
3-(Chloromethylthio)toluene (6.5 mmol) was added to a solution of 5-fluoropyrimidin-2-one (6.5 mmol) and triethylamine (6.5 mmol) in dichloromethane (75 ml) and the resultant mixture heated under reflux for 2 days. The solvent was then distilled off, the residue triturated with water and the residual material extracted with CCl4. Evaporation of the extracts and crystallisation of the residue from ethyl acetate gave the pure product; 0.40 g (25%), m.p. 124° C. (Found: C57.42; H4.63. Calc. for C12H11FN2OS: C57.59; H4.43) 1H NMR (DMSO d6); δ 2.28 (Me), 5.17(CH2), 7.2 (Ph), 8.05 (H-4), 8.70 (H-6). IR (KBr): 1670 cm-1 (CO), MS [70 eV, m/z (% rel. int.)]: 250 (8,M), 137(11), 136)36), 135(10), 128(7), 127(100), 100(34), 91(9).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04596870 |
| Quelldatensatz | uspto-grants-1986_06 |
| ORD ID | ord-229255d0db2347b2bea28eaa4d01f0b9 |
| Quellennotiz | uspto-grants-1986_06 |