HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Mercaptoethanol → 2-[(3,6-Dichloro-4-pyridazinyl)thio]ethanol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Mercaptoethanol | HCID 1567 | — |
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | 3,4,6-Trichloropyridazine | HCID 95123 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Triethylamine | HCID 8471 | — |
| Produkt | 2-[(3,6-Dichloro-4-pyridazinyl)thio]ethanol | HCID 81766083 | — |
Reaktionsschritte
A solution of 3,4,6-trichioropyridazine (25 g) in tetrahydrofuran (200 ml) and triethylamine (19 ml) was treated at 0° C. (ice bath cooling) with 2-mercaptoethanol (8.33 ml) over 5 minutes. After the addition was complete, the mixture was stirred at room temperature for 72 hours. The mixture was stirred with aqueous sodium bicarbonate solution and dichloromethane and the solid was collected, washed with water, ether and pentane and dried in vacuo, giving (22.9 g). The combined aqueous and organic fraction was evaporated to half volume giving further solid, which was washed and dried as above (5.0 g). The total yield of solid (27.9 g; 91%) contained some bromo-analogue (5-10%) by NMR.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07732460B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-ac95521bbf7746a397c2d885666fc1aa |
| Quellennotiz | uspto-grants-2010_06 |