HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 10065497, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Ethylimidazole | HCID 66130 | — |
| Reactant | 6-Methylergolin-8beta-ylmethyl tosylate | HCID 13933015 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10065497 | HCID 10065497 | 61.4% |
Reaction Steps
0.9 g of 50% sodium hydride in an oil was added in small portions to a mixture of 3.0 g of 2-ethylimidazole and 60 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 3.0 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 1.5 hours. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluted with acetone). The product was recrystallized from methanolisopropyl alcohol to obtain 1.5 g of the titled compound having a melting point of 232°-237° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04713457 |
| Source dataset | uspto-grants-1987_12 |
| ORD ID | ord-340c671d331a44bfa8fcd96b92fa2bc1 |
| Source note | uspto-grants-1987_12 |