HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methylimidazole → HCID 10403745, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methylimidazole | HCID 12749 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 6-Methylergolin-8beta-ylmethyl tosylate | HCID 13933015 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10403745 | HCID 10403745 | 70.5% |
Reaction Steps
0.8 g of 50% sodium hydride in an oil was added in small portions to a mixture of 1.2 g of 2-methylimidazole and 16 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 2.0 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 3 hours. After allowing the mixture to cool, ice-water was added to the reaction mixture, and the precipitated crystals were separated by filtration, washed with water and purified by silica gel column chromatography (eluted with chloroform). The product was recrystallized from ethanol to obtain 1.1 g of the titled compound as colorless needles having a melting point higher than 300° C. (with decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04713457 |
| Source dataset | uspto-grants-1987_12 |
| ORD ID | ord-effd959f48cd4da9811c210bdd849ea1 |
| Source note | uspto-grants-1987_12 |