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Phosphorus oxychloride → 5-methyl-7-[3-(trifluoromethyl)phenyl]-N-(3,4,5-trimethoxyphenyl)imidazo[5,1-f][1,2,4]triazin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3-(trifluoromethyl)-N-(1-{3-[(3,4,5-trimethoxyphenyl)amino]-1,2,4-triazin-6-yl}ethyl)benzamide | HCID 58711986 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 5-methyl-7-[3-(trifluoromethyl)phenyl]-N-(3,4,5-trimethoxyphenyl)imidazo[5,1-f][1,2,4]triazin-2-amine | HCID 11328632 | 3.3% |
反応手順
In a similar manner as described for Example 1, 3-(trifluoromethyl)-N-(1-{3-[(3,4,5-trimethoxyphenyl)amino]-1,2,4-triazin-6-yl}ethyl)benzamide (Intermediate 14) (0.12 g, 0.25 mmol) in 1,2-dichloroethane (20 mL) and phosphorus oxychloride (0.28 mL, 3.0 mmol) gave 5-methyl-7-[3-(trifluoromethyl)phenyl]-N-(3,4,5-trimethoxyphenyl)imidazo[5,1-f][1,2,4]triazin-2-amine (0.0038 g) as a yellow solid. 1H NMR (CD3OD): δ9.08 (s, 1H), 8.72 (d, J=7.7 Hz, 1H), 8.59 (s, 1H), 7.76-7.65 (m, 2H), 7.00 (s, 2H), 6.99 (s, 1H), 3.76 (s, 3H), 3.74 (s, 6H), 2.60 (s, 3H). MS m/z 460 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07462614B2 |
| 出典データセット | uspto-grants-2008_12 |
| ORD ID | ord-cbdf8b4150f84ccc851d9d0d4c213c17 |
| 出典メモ | uspto-grants-2008_12 |