HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,2-Dimethoxyethane → Ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2]bipyrimidinyl-4-yl]-amide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,2-Dimethoxyethane | HCID 8071 | — |
| Edukt | Potassium tert-butoxide | HCID 23665647 | — |
| Edukt | Ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-[2,2']bipyrimidinyl-4-yl]-amide | HCID 59645271 | — |
| Lösungsmittel | Ethylene Glycol | HCID 174 | — |
| Produkt | Ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2]bipyrimidinyl-4-yl]-amide | HCID 59645268 | — |
Reaktionsbedingungen
| Temperatur | 85 °C |
|---|
Reaktionsschritte
To a solution of potassium tert.-butoxide (366.5 mg) in ethylene glycol (5 ml) was added 1,2-dimethoxy ethane (5 ml) and ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidinyl-4-yl]-amide (420 mg). The reaction mixture was heated to 85° C. for 7 days, concentrated in vacuo, poured onto water, acidified by 2N HCl, and extracted with ethyl acetate. The combined organic extracts were dried over magnesium sulfate and concentrated in vacuo. The precipitated product was washed with diethyl ether, filtered and dried at HV to give ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidinyl-4-yl]-amide (400 mg). LC-MS: tR: 3.45, [M+H]+: 448.24.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07323465B2 |
| Quelldatensatz | uspto-grants-2008_01 |
| ORD ID | ord-daca05c35a284770ab324c5d6ee82d46 |
| Quellennotiz | uspto-grants-2008_01 |