Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cabergoline | HCID 54746 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 69068522 | HCID 69068522 | 403.6% |
Reaction Steps
The oil obtained by purification on a chromatographic column after the final step of the synthetic path according to the preparation described in Eur. J. Med. Chem., 24, 421, (1989) and containing 100 g of pure cabergoline was dissolved in toluene to give 243 g of a cabergoline toluene solution. The solution was introduced into a reactor pre-cooled at −12° C., and 182 g of toluene were added to give a 23.5%. w/w cabergoline concentration in this solvent. After cooling again at −12° C., 362 ml of diethyl ether were added. The mixture was cooled again at −12° C. and stirred at this temperature for about 17 hours. The obtained precipitate was filtered under vacuum and smoothly dried. The resultant crystal solvate form V was identified by XRD, DSC, IR and NMR, data shown in FIGS. 5-8 respectively.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06727363B2 |
|---|
| Source dataset | uspto-grants-2004_04 |
|---|
| ORD ID | ord-eda90de97333469582864d5d4db451f5 |
|---|
| Source note | uspto-grants-2004_04 |
|---|