HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → 5-Trifluoromethyl-2-{4-[(6-trifluoromethyl-pyridin-3-ylmethyl)-amino]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl}-benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Fluoro-5-(trifluoromethyl)benzonitrile | HCID 521016 | — |
| 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 | 5-Trifluoromethyl-2-{4-[(6-trifluoromethyl-pyridin-3-ylmethyl)-amino]-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl}-benzonitrile | HCID 25061874 | — |
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 (40 mg, 0.13 mmol), 2-fluoro-5-(trifluoromethyl)benzonitrile (150 mg, 0.78 mmol), acetonitrile (0.4 mL) and N,N-diisopropylethylamine (68 μL, 0.39 mmol). The mixture was subjected to microwave irradiation at 200° C. for 2 h. 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 silica gel column to yield a pale brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076345B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-4c8861b155554241bc290520e36967b8 |
| Source note | uspto-grants-2011_12 |