HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → 1-(6-Methylergolin-8beta-ylmethyl)tetrazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 6-Methylergolin-8beta-ylmethyl tosylate | HCID 13933015 | — |
| Reactant | HCID 178418441 | HCID 178418441 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-(6-Methylergolin-8beta-ylmethyl)tetrazole | HCID 10040940 | 31.1% |
Reaction Steps
1.7 g of 50% sodium hydride in an oil was added in small portions to a mixture of 5.1 g of tetrazole and 30 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 11 hours. The solvent was distilled off under reduced pressure, and the residue was purified by alumina column chromatography (eluted with acetone). The product was recrystallized from acetone to obtain 0.7 g of the titled compound as colorless needles having a melting point of 206°-209° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04713457 |
| Source dataset | uspto-grants-1987_12 |
| ORD ID | ord-9a29efd8a44a41c994139f5995a3a73f |
| Source note | uspto-grants-1987_12 |