HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → (5R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methyl)amino]-4-(4-fluoro-2-methylphenyl)-2-pyridinyl]-2-methyl-D-prolinamide citrate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | (5R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methyl)amino]-4-(4-fluoro-2-methylphenyl)-2-pyridinyl]-2-methyl-D-prolinamide | HCID 44472503 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | (5R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methyl)amino]-4-(4-fluoro-2-methylphenyl)-2-pyridinyl]-2-methyl-D-prolinamide citrate | HCID 86636102 | — |
Reaction Steps
25 mg of (5R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methy)amino]-4-(4-fluoro-2-methylphenyl)-2-pyridinyl]-2-methyl-D-prolinamide (Example 1) were dispensed into a HPLC vial followed by 7.6 mg (1 eq) citric acid. 250 μL of toluene were then dispensed on to the solid and the reaction was set to temperature cycle (0-40° C.) whilst stirring at 500 rpm. After 2.5 days, the solid was isolated by filtration at ambient. Onset melt ca.90° C. by DSC followed by decomposition.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822504B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-4f9d87b1baf54162b16922ec3bb1320e |
| Source note | uspto-grants-2014_09 |