HuagongsheHuagongshe Chemistry Print Report · For research reference only
Fumaric Acid → (R)-2-(1,2-dihydroxypropan-3-ylamino)-8-isopropyl-4-[4-(pyridin-2-yl)benzylamino]pyrazolo[1,5-a]-1,3,5-triazine fumarate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | (R)-2-(1,2-dihydroxypropan-3-ylamino)-8-isopropyl-4-[4-(pyridin-2-yl)benzylamino]pyrazolo[1,5-a]-1,3,5-triazine | HCID 46910677 | — |
| Solvent | Diethyl ether ethanol | HCID 21585056 | — |
| Product | (R)-2-(1,2-dihydroxypropan-3-ylamino)-8-isopropyl-4-[4-(pyridin-2-yl)benzylamino]pyrazolo[1,5-a]-1,3,5-triazine fumarate | HCID 46910763 | — |
Reaction Steps
The product 10 is treated with fumaric acid in an EtOH/Et2O solution. The fumaric acid salt 11 crystallizes from the reaction medium. Mp=168-170° C. 1H NMR (300 MHz, CDCl3 1 drop DMSO-d6): δ 8.64 (d, 1H, J=3.8 Hz, Harom), 7.93 (d, 2H, J=8.1 Hz, Harom), 7.74-7.65 (m, 2H, Harom), 7.60 (s, 1H, Harom), 7.42 (d, 2H, J=8.1 Hz, Harom), 7.26-7.18 (m, 1H, Harom), 6.76 (s, 2H, ═CH), 4.74 (d, 2H, J=5.9 Hz, CH2), 3.80-3.75 (m, 1H, CH), 3.56-3.45 (m, 4H, 2 CH2), 2.99 (hept, 1H, J=6.8 Hz, CH), 1.23 (d, 6H, J=6.8 Hz, 2 CH3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08691982B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-8f6d134a652c4546be1360f904c6af2a |
| Source note | uspto-grants-2014_04 |