HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 131715472, compound → HCID 131715474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 131715472 | HCID 131715472 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Chloride | HCID 5234 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131715474 | HCID 131715474 | 68.4% |
Reaction Steps
Under argon, 183 mg (0.39 mmol) of 3-[1-(tertbutyldimethylsilyl)-9,10-didehydro-2,6-dimethyl-8α-ergolinyl]-1,1-diethylurea is dissolved in 5 ml of methanol with addition of 2 ml of tetrahydrofuran and stirred with 1 ml of 14N potassium hydroxide solution at room temperature for 17 hours. To work up the mixture, it is diluted with saturated sodium chloride solution and extracted with methylene chloride. The methylene chloride extracts are washed with saturated sodium chloride solution and water and dried over sodium sulfate. The crude product of 128 mg is chromatographed and crystallized as the tartrate, thus obtaining 94 mg (67% of theory) of 3-(9,10-didehydro-2,6-dimethyl-8α-ergolinyl)-1,1-diethylurea.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04731367 |
| Source dataset | uspto-grants-1988_03 |
| ORD ID | ord-3d81b8ba5a0e487c8bdfcedc20235d54 |
| Source note | uspto-grants-1988_03 |