HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formamidine acetate → HCID 51353438, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formamidine acetate | HCID 160693 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | HCID 86652979 | HCID 86652979 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 51353438 | HCID 51353438 | 4% |
Reaction Steps
N-{2-[5-cyclopropyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]pyrimidin-5-yl}-2-[(dimethylamino)methylene]-3-oxobutanamide (0.3 g, 0.78 mmol) and formamidine acetate (98 mg, 0.94 mmol) were dissolved in ethanol and added NaOEt (60 mg, 0.94 mmol). The above mixture was refluxed for 3 h. Ethanol was removed on rotavapour and worked up (H2O/AcOEt) to obtain the crude. Crude was purified by column on 60-120 mesh silica gel using AcOEt and Petether (1:1) as eluent to obtain the title compound (12 mg) as a brown solid. M.P.: 201-203° C. 1H-NMR (δ ppm, DMSO-d6, 400 MHz): 11.29 (s, 1H), 9.26 (s, 2H), 9.19 (s, 1H), 8.99 (s, 1H), 6.68 (s, 1H), 2.64 (s, 3H), 2.55-2.49 (m, 1H), 1.02-0.94 (m, 2H), 0.83-0.75 (m, 2H). MS (m/z): 389.93 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921364B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-160684e6506a4aaabe42e83aa5958a8a |
| Source note | uspto-grants-2014_12 |