関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosgeniminium chloride | HCID 2723945 | — |
| 反応物 | 7-(3,5-dimethylisoxazol-4-yl)-6-methoxy-N4-((tetrahydro-2H-pyran-4-yl)methyl)quinoline-3,4-diamine | HCID 70981155 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 66571468 | HCID 66571468 | 77.1% |
反応手順
7-(3,5-Dimethylisoxazol-4-yl)-6-methoxy-N4-((tetrahydro-2H-pyran-4-yl)methyl)quinoline-3,4-diamine (for preparation see intermediate 17) (50 mg, 0.131 mmol) and N-(dichloromethylene)-N-methylmethanaminium chloride (available from Aldrich) (42.5 mg, 0.261 mmol) were combined in anhydrous acetonitrile (0.5 ml) and heated at 120° C. for 10 min (microwave). The reaction mixture was reduced to dryness under a stream of nitrogen and the residue dissolved in DMSO (1 ml) and purified by MDAP (HpH). The solvent was evaporated under a stream of nitrogen to give 7-(3,5-dimethylisoxazol-4-yl)-8-methoxy-N,N-dimethyl-1-((tetrahydro-2H-pyran-4-yl)methyl)-1H-imidazo[4,5-c]quinolin-2-amine (44 mg, 0.101 mmol, 77% yield) as a yellow gum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846709B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-bf9b80d969764afb86a5549be39dc58b |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|