HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,3-Dichloropropane → 2-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide Ethylene Ketal
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,3-Dichloropropane | HCID 8881 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide ethylene ketal | HCID 21817893 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide Ethylene Ketal | HCID 12111731 | 84,4% |
Reaktionsschritte
To a suspension of 2.20 g (50 mmol) of 60% sodium hydride in 100 ml of DMF, a solution of 12.06 g (50 mmol) of 3,4-dihydro-2H-1,2-benzothiazin-4-one 1,1-dioxide ethylene acetal in 50 ml of DMF was added under ice cooling and stirring. The reaction mixture was stirred for 30 minutes at 0° C. and then for further one hour at room temperature. Under ice cooling, a solution of 16.95 g (150 mmol) of 1,3-dichloropropane in 50 ml of DMF was added to the reaction mixture, followed by stirring for 17 hours at room temperature. The post-treatment and purification were conducted as in Example 10, whereby 13.41 g of the title compound were obtained (yield: 84%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05874429 |
| Quelldatensatz | uspto-grants-1999_02 |
| ORD ID | ord-20b95a6ce7b8435285369d52bab50899 |
| Quellennotiz | uspto-grants-1999_02 |