HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 60204316, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 60204300 | HCID 60204300 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 60204316 | HCID 60204316 | 73.7% |
Reaction Steps
1-(2-(4-(4,5-Dichlorothiophen-2-yl)pyrimidin-2-ylamino)ethyl)-5,5-dimethyl imidazolidine-2,4-dione (300 mg, 0.75 mmol) was suspended in a 10% solution of methanol in dichloromethane (7 mL). Glacial acetic acid (1 mL) followed by bromine (120 mg, 0.75 mmol, 39 μL) [material immediately went into solution] were added, and the mixture was stirred at room temperature for 3 h. The reaction was concentrated in vacuo, diluted with deionized water (25 mL), stirred for 5 min, and then the product was collected by filtration to give a yellow solid (265 mg). The crude product was purified by flash chromatography (MeOH/DCM) to yield the title compound as a yellow powder (162 mg, 45%). MS (M+H)+ 478/480.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07858785B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-a674079645b14e4493bb0e48954848ad |
| Source note | uspto-grants-2010_12 |