Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | HCID 58266282 | HCID 58266282 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58266267 | HCID 58266267 | — |
Reaction Steps
527 mg (1.0 mmol) of ethyl 4-(4-cyanophenyl)-1-[4-fluoro-3-(trifluoromethyl)phenyl]-6-(bromomethyl)-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate were dissolved in 25 ml of dioxane, and 138 mg (3.0 mmol; 3 eq.) of methylhydrazine were added. The mixture was stirred at 120° C. for 1 h and then concentrated. The residue was purified directly by preparative HPLC (column: Gromsil C-18 10 μm; mobile phase: acetonitrile/water+0.1% TFA 10:90→90:10). This gave 270 mg (55% of theory) of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08580800B2 |
|---|
| Source dataset | uspto-grants-2013_11 |
|---|
| ORD ID | ord-f384ace35a394900868b4121391e9a07 |
|---|
| Source note | uspto-grants-2013_11 |
|---|