HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,2-Dichloroethane → 4-chloro-N-methylbenzothiazolone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,2-Dichloroethane | HCID 11 | — |
| Edukt | Dimethyl Sulfate | HCID 6497 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 4-Chlorobenzothiazolone | HCID 53400688 | — |
| Katalysator | Tetrabutylammonium Bromide | HCID 74236 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-chloro-N-methylbenzothiazolone | HCID 69645010 | 93,9% |
Reaktionsschritte
4-Chlorobenzothiazolone (9.28 g, 0.05 mole) was dissolved in a solution of sodium hydroxide (3.19 g, 0.075 mole) in water (500 ml), and tetra-n-butylammonium bromide (0.48 g, 0.0015 mole) and ethylene dichloride (300 ml) were added thereto. Dimethyl sulfate (9.40 g, 0.075 mole) was added dropwise thereto at room temperature, and the mixture was stirred at room temperature for 1 hour, followed by phase-separation. The ethylene dichloride layer was washed once with water, and the solvent was removed under reduced pressure to obtain 9.37 g of 4-chloro-N-methylbenzothiazolone as pale yellow crystals. Yield 93.9%, purity 98.7%, m.p. 130°-132° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04293702 |
| Quelldatensatz | uspto-grants-1981_10 |
| ORD ID | ord-5d1e1d871b804ddda12daf9877af0ddf |
| Quellennotiz | uspto-grants-1981_10 |