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1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene → 1-[3-(4-Bromo-2-methyl-2H-pyrazol-3-yl)-4-methoxy-phenyl]-3-(4-Chloro-3-trifluoromethyl-phenyl)-urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene | HCID 2733265 | — |
| 反応物 | 3-(4-Bromo-1-methyl-1H-pyrazol-5-yl)-4-methoxyaniline | HCID 11572741 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[3-(4-Bromo-2-methyl-2H-pyrazol-3-yl)-4-methoxy-phenyl]-3-(4-Chloro-3-trifluoromethyl-phenyl)-urea | HCID 11519011 | 83.3% |
反応手順
3-(4-Bromo-2-methyl-2H-pyrazol-3-yl)-4-methoxy-phenylamine (0.035 g, 0.12 mmol) was treated with 4-chloro-3-(trifluoromethyl)phenyl isocyanate (0.027 g, 0.12 mmol, 1.0 equiv.) in CH2Cl2 (2 mL), in a similar manner as described in Example 1.2 to afford Compound 6 (0.051 g, 0.10 mmol, 81%) as a white solid. LCMS m/z (%)=503 (M+H79Br35Cl, 78), 505 (M+H81Br35Cl, 100), 507 (M+H81Br37Cl, 28). 1H NMR (400 MHz, acetone-d6) δ: 8.52 (s, 1H), 8.27 (s, 1H), 8.13 (s, 1H), 7.74 (b, J=8.7 Hz, 1H), 7.68 (d, J=9.0 Hz, 1H), 7.53 (d, J=8.7 Hz, 1H), 7.49 (s, 1H), 7.43 (s, 1H), 7.14 (d, J=9.0 Hz, 1H), 3.82 (s, 3H), 3.68 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754238B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-445cba3de6554bd19b0eedc302c5af43 |
| 出典メモ | uspto-grants-2014_06 |