HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl Sulfide → 3-(6-Methyl-13-nitro-8beta-ergolinyl)-1,1-diethylurea
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl Sulfide | HCID 1068 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Tert-Butyl hypochlorite | HCID 521297 | — |
| Edukt | Sodium ethoxide | HCID 2723922 | — |
| Edukt | 3-(2,3-Dihydro-6-methyl-13-nitro-8beta-ergolinyl)-1,1-diethylurea | HCID 86742352 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 3-(6-Methyl-13-nitro-8beta-ergolinyl)-1,1-diethylurea | HCID 86742351 | 25,9% |
Reaktionsschritte
A solution of 0.4 mmol of tert-butyl hypochlorite in 2 ml of methylene chloride is added dropwise to a solution of 0.3 mmol of 3-(2,3-dihydro-6-methyl-13-nitro-8β-ergolinyl)-1,1-diethylurea, 0.4 mmol of dimethyl sulfide, and 0.3 mmol of triethylamine in 5 ml of methylene choride at -70° C., and the mixture is agitated for 2 hours. Then a solution of 2 mmol of sodium ethylate in 2 ml of ethanol is added thereto within 10 minutes, and the mixture is warmed up to room temperature within 2 hours, whereafter it is combined with water, extracted with methylene chloride, the organic phase is dried and evaporated. Chromatography on silica gel with methylene chloride/methanol (5%) yields 30 mg of 3-(6-methyl-13-nitro-8β-ergolinyl)-1,1-diethylurea.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04766128 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-b8a17eee9b8649738d7245eacbbd1a9e |
| Quellennotiz | uspto-grants-1988_08 |