HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → 3-[3-(Dichloromethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Lithium Chloride | HCID 433294 | — |
| Edukt | 3-[3-(dibromomethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 22119839 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 3-[3-(Dichloromethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 22119982 | — |
Reaktionsschritte
A solution of 3-[3-(dibromomethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (0.750 g, 0.00150 mol) and lithium chloride (0.950 g, 0.0225 mol) in N,N-dimethylformamide is stirred at room temperature for 48 hours and diluted with ethyl acetate. The resultant mixture is washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a foam. Column chromatography of the foam using silica gel, methylene chloride, and a 1% diethyl ether in methylene chloride solution gives the title product as a white foam (0.530 g, mp 148-149° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06156700 |
| Quelldatensatz | uspto-grants-2000_12 |
| ORD ID | ord-c60fa8a7f7df48388eee992be0e39f14 |
| Quellennotiz | uspto-grants-2000_12 |