HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanesulfonylchloride, 2-chloro- → 9-[4-(3-Methylphenoxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 3-(4-(3-Methylphenoxy)phenyl)pyridin-2-amine | HCID 66747992 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 9-[4-(3-Methylphenoxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide | HCID 66748857 | — |
Reaktionsschritte
To a suspension of NaH (60%, 370 mg) in THF (dry) (25 mL) was added 2-chloroethanesulfonyl chloride (0.583 mL) at 0° C. and the mixture was stirred for 5 min at the same temperature. A solution of 3-(4-(3-methylphenoxy)phenyl)pyridin-2-amine (511 mg) in THF (dry) (40 mL) was added at 0° C. and the mixture was stirred at room temperature overnight. The mixture was quenched with water at 0° C. Water, EtOAc and IPE were added and the precipitates were collected, washed with water/EtOAc, dried in vacuo to give the title compound (514 mg) as a white solid. A part of this was recrystallized from MeCN/IPE.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08575154B2 |
| Quelldatensatz | uspto-grants-2013_11 |
| ORD ID | ord-31d4c41001d1496bbf8f04acbef68ec1 |
| Quellennotiz | uspto-grants-2013_11 |