HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4,6-Dichloro-n-methylpyrimidin-2-amine → 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4,6-Dichloro-n-methylpyrimidin-2-amine | HCID 259880 | — |
| Edukt | 4-Chloro-benzenesulfonamide potassium salt | HCID 131721322 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide | HCID 19353555 | 85% |
Reaktionsschritte
0.39 g (0.0022 mol) of (4,6-dichloro-pyrimidin-2-yl)-methylamine and 1.0 g (0.0044 mol) of 4-chloro-benzene-sulfonamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 150° C. for 8 hours. Then, the solvent was distilled off in a high vacuum, the residue was partitioned in ethyl acetate/water and extracted. The aqueous phase was saturated with sodium chloride, evaporated briefly in a vacuum, made acid with 4N HCl and extracted with dichloromethane. The two extracts were combined and chromatographed over silica gel with cyclohexane/ethyl acetate 1:1 as the eluent. There was obtained 0.62 g (85%) of 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide as white crystals. m.p. 196-198° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06030976 |
| Quelldatensatz | uspto-grants-2000_02 |
| ORD ID | ord-94ca1704d3754db286060055fdd4c10c |
| Quellennotiz | uspto-grants-2000_02 |