HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 25062143, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,5-Difluorobenzonitrile | HCID 123558 | — |
| Reactant | N-((6-(trifluoromethyl)pyridin-3-yl)methyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine | HCID 59840682 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 25062143 | HCID 25062143 | 11.7% |
Reaction Steps
A 2 mL microwave vial was charged with N-((6-(trifluoromethyl)pyridin-3-yl)methyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (50 mg, 0.16 mmol), 2,5-difluorobenzonitrile (130 mg, 0.97 mmol), acetonitrile (0.4 mL) and N,N-diisopropylethylamine (84 μL, 0.48 mmol). The mixture was subjected to microwave irradiation at 200° C. for 4 h. After cooling the mixture was diluted with chloroform (7 mL), and washed with 0.1 M NaH2PO4 (10 mL), dried (Na2SO4), filtered and concentrated. The residue was purified by semi-preparative HPLC (100×20.2 mm, C18 column; 20-90% MeCN/H2O [10 mM diethylamine]) to yield an off-white solid (8 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076345B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-37d5856ea2e24f42a8128731a85bd92f |
| Source note | uspto-grants-2011_12 |