HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 8-[1-(Pyridin-3-yl)vinyl]-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Methyl chlorosulphate | HCID 69938 | — |
| Edukt | 1-(10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)1-(pyridin-3-yl)ethanol | HCID 18670441 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 8-[1-(Pyridin-3-yl)vinyl]-10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine | HCID 18670322 | 79,8% |
Reaktionsschritte
To a solution of 303 mg of 1-(10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)1-(pyridin-3-yl)ethanol in dichloromethane was added in a nitrogen atmosphere 0.32 ml of methyl chlorosulfonate and the resulting mixture was heated under reflux for 2 hours. Then the reaction mixture was brought back to room temperature and distributed into water and ethyl acetate. The extract was dried over anhydrous magnesium sulfate and filtered. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 230 mg of the title compound as a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06518423B1 |
| Quelldatensatz | uspto-grants-2003_02 |
| ORD ID | ord-03dc200643aa4ec2bda2b17c98c9faf0 |
| Quellennotiz | uspto-grants-2003_02 |