関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-(Trifluoromethyl)aniline | HCID 6922 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 7-Amino-4-methylthiopyrido[4,3-d]pyrimidine | HCID 10442562 | — |
| 反応物 | Alpha,alpha,alpha-trifluoro-O-toluidine hydrochloride | HCID 22736790 | — |
| 溶媒 | Chloroform methanol | HCID 21584188 | — |
| 生成物 | 4-N-[2-(trifluoromethyl)phenyl]pyrido[4,3-d]pyrimidine-4,7-diamine | HCID 5328057 | 41% |
反応手順
A mixture of 7-amino-4-methylthiopyrido[4,3-d]pyrimidine (300 mg, l.56 mmol), 2-aminobenzotrifluoride hydrochloride (1.00 g, 5.06 mmol) and 2-aminobenzotrifluoride (2.00 g, 12.4 mmol) is stirred at 160° C. for 10 min. The resulting product is neutralized with excess NaHCO3, dissolved in MeOH/CHCl3, dried onto silica gel and chromatographed over silica gel (6-7%; MeOH/CH2Cl2) to give 7-amino-4-(2-trifluoromethylanilino)pyrido[4,3-d]pyrimidine (194 mg, 41%) as a cream solid, mp (MeOH/CHCl3/light petroleum) 126-130 ° C. (dec.). 1H NMR (DMSO) δ 10.60 (1H, brs), 9.17 (1H, brs), 8.13 (1H, brs), 7.76, 7.69 (1H, 1H, m, m), 7.45 (2H, m), 6.66 (2H, brs), 6.36 (1H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06713484B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-9e6104713dad4b338ddb9caf5642ed6c |
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| 出典メモ | uspto-grants-2004_03 |
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