HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trichloromethanethiol → 4-(5-Chloro-1,2,4-thiadiazol-3-yl)morpholine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trichloromethanethiol | HCID 6390 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Morpholine-4-carboximidamide Hydrobromide | HCID 2806564 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-(5-Chloro-1,2,4-thiadiazol-3-yl)morpholine | HCID 56832319 | 54,6% |
Reaktionsschritte
To a solution of morpholinoformamidine hydrobromide (2.00 g, 9.52 mmol) and perchloromethyl mercaptan (1.02 ml, 9.52 mmol) in dichloromethane (10 ml) was added dropwise a solution of sodium hydroxide (1.52 g, 38.1 mmol) in water (4 ml) under ice-cooling. Then, the reaction mixture was stirred under ice-cooling for 1 hour and at room temperature for 1 hour. The organic layer was separated, washed with water, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to give 1.07 g (54.6%) of the desired product as a solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07851473B2 |
| Quelldatensatz | uspto-grants-2010_12 |
| ORD ID | ord-0ea681c1103c43bc8ab92d6920fb398c |
| Quellennotiz | uspto-grants-2010_12 |