HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trichloroisocyanuric Acid | HCID 6909 | — |
| Reactant | 3-(2-Bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea | HCID 13059860 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | 3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea | HCID 67788573 | — |
Reaction Steps
2.1 g of 3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea (5 mmol) and 388 mg of trichloroisocyanuric acid (1.67 mmol) are dissolved in 100 ml of trifluoroacetic acid at room temperature. After 15 minutes, ice is added, it is made alkaline with conc. ammonia and shaken out with dichloromethane. The organic phases are dried and concentrated by evaporation, the residue is chromatographed and the product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05411966 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-e4f87c257b9c434bb882cda9bcf99f6e |
| Source note | uspto-grants-1995_05 |