HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Oxalic Acid → 4-(N-allyl-N-methylaminoacetyl)-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine oxalate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Oxalic Acid | HCID 971 | — |
| Edukt | Allyl bromide | HCID 7841 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-(4-chlorophenyl)-4-(N-methylaminoacetyl)-3,4-dihydro-2H-1,4-benzothiazine | HCID 18984435 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-(N-allyl-N-methylaminoacetyl)-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine oxalate | HCID 18984433 | — |
Reaktionsschritte
A mixture of 2-(4-chlorophenyl)-4-(N-methylaminoacetyl)-3,4-dihydro-2H-1,4-benzothiazine (1.80 g), allyl bromide (0.52 ml), potassium carbonate (2.25 g) and dimethylformamide (20 ml) is stirred at room temperature for 3.5 hours. The reaction mixture is poured into water, and the mixture is extracted with ethyl acetate. After the solvent is distilled off, the residue is purified by silica gel column chromatography (solvent, chloroform:methanol=40:1). The caramel thus obtained is dissolved in ether and thereto is added 1.1 equivalent of oxalic acid. The resulting precipitate is washed with ether and dried to give 4-(N-allyl-N-methylaminoacetyl)-2-(4-chlorophenyl)-3,4-dihydro-2H-1,4-benzothiazine oxalate as powder.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05246929 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-95b2bc44ff6d4a949fc4fdaff92f4f93 |
| Quellennotiz | uspto-grants-1993_09 |