関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Picolinic acid | HCID 1018 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 反応物 | 8-amino-3-methyl-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one | HCID 58552822 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-methyl-4-oxo-2-(3-(trifluoromethyl)phenyl)-3,4-dihydroquinazolin-8-yl)picolinamide | HCID 45255149 | 93% |
反応手順
A mixture of 8-amino-3-methyl-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one 5 (106 mg, 0.33 mmol), pyridine-2-carboxylic acid 6 (84 mg, 0.68 mmol), HATU (263 mg, 0.69 mmo) and DIPEA (208 mg) in DMF were heated at 55° C. for 2.5 h then poured into H2O. The resulting precipitate was collected by filtration, rinsed with H2O, then Et2O to give Compound 239 as a yellow solid (130 mg, 93% yield). MS (ESI) calc. for C22H15F3N4O2: 424.11. found: 425 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09326986B2 |
|---|
| 出典データセット | uspto-grants-2016_05 |
|---|
| ORD ID | ord-50d484079dd847f5b3902c0eeb4e7211 |
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| 出典メモ | uspto-grants-2016_05 |
|---|
